# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2H
_database_code_depnum_ccdc_archive 'CCDC 2335829'
loop_
_audit_author_name
_audit_author_address
'Mirta Rubcic'
;University of Zagreb
Croatia
;
_audit_update_record             
;
2024-02-27 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-04-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Mo6 O19, 2(C14 H12 Mo N3 O5)'
_chemical_formula_sum            'C28 H24 Mo8 N6 O29'
_chemical_formula_weight         1676.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Mo8 C26 N6 O27'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8506(5)
_cell_length_b                   9.2538(5)
_cell_length_c                   14.0175(8)
_cell_angle_alpha                74.262(5)
_cell_angle_beta                 72.168(5)
_cell_angle_gamma                88.125(4)
_cell_volume                     1050.34(11)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    8984
_cell_measurement_temperature    170
_cell_measurement_theta_max      79.3820
_cell_measurement_theta_min      3.3430
_shelx_estimated_absorpt_T_max   0.826
_shelx_estimated_absorpt_T_min   0.267
_exptl_absorpt_coefficient_mu    19.916
_exptl_absorpt_correction_T_max  0.04478
_exptl_absorpt_correction_T_min  0.00174
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.650
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       sphere
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_exptl_crystal_size_rad          0.400
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13693
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.012
_diffrn_reflns_theta_min         3.444
_diffrn_ambient_temperature      170
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     97.00 141.00   0.50    0.12    --  113.25  61.00   0.00   88
  2  ω    147.00 173.00   0.50    0.12    --  113.25  61.00   0.00   52
  3  ω    102.00 154.00   0.50    0.12    --  113.25  56.00-103.00  104
  4  ω     99.00 171.00   0.50    0.12    --  113.25  61.00-180.00  144
  5  ω     87.00 119.00   0.50    0.05    --   47.77  56.00-103.00   64
  6  ω    108.00 169.00   0.50    0.12    --  113.25  45.00 -30.00  122
  7  ω    143.00 169.00   0.50    0.12    --  113.25  45.00  60.00   52
  8  ω    153.00 178.00   0.50    0.12    --  113.25  15.00 120.00   50
  9  ω    101.00 149.00   0.50    0.12    --  113.25  15.00 120.00   96
 10  ω    102.00 174.00   0.50    0.12    --  113.25  45.00 150.00  144
 11  ω    107.00 157.00   0.50    0.12    --  113.25 125.00 -90.00  100
 12  ω    145.00 178.00   0.50    0.12    --  113.25 125.00-120.00   66
 13  ω     96.00 169.00   0.50    0.12    --  113.25 125.00-180.00  146
 14  ω     95.00 134.00   0.50    0.12    --  113.25 125.00-120.00   78
 15  ω    137.00 163.00   0.50    0.12    --  113.25 125.00 150.00   52
 16  ω    -71.00 -22.00   0.50    0.12    --  -91.75  61.00  90.00   98
 17  ω    -51.00 -25.00   0.50    0.12    --  -91.75  45.00   0.00   52
 18  ω    -11.00  24.00   0.50    0.05    --  -47.77  56.00-103.00   70
 19  ω    -61.00 -14.00   0.50    0.05    --  -47.77  56.00-103.00   94
 20  ω    -53.00 -21.00   0.50    0.12    --  -91.75  56.00-103.00   64
 21  ω   -119.00 -34.00   0.50    0.05    --  -47.77 -56.00 114.00  170
 22  ω   -160.00-116.00   0.50    0.12    --  -91.75 -56.00 114.00   88
 23  ω   -111.00 -73.00   0.50    0.05    --  -47.77-125.00  60.00   76
 24  ω    -26.00  15.00   0.50    0.05    --   47.77 -19.00  30.00   82
 25  ω    -23.00   3.00   0.50    0.05    --   47.77 -56.00 114.00   52
 26  ω    -21.00  26.00   0.50    0.05    --   47.77 -19.00 120.00   94
 27  ω     28.00  53.00   0.50    0.05    --   47.77 -56.00 114.00   50
 28  ω     56.00  82.00   0.50    0.12    --  113.25-136.00  44.35   52
 29  ω     95.00 120.00   0.50    0.12    --  113.25-136.00  44.35   50
 30  ω     51.00 111.00   0.50    0.12    --  113.25-125.00  60.00  120
 31  ω     81.00 110.00   0.50    0.12    --  113.25-125.00  90.00   58
 32  ω     45.00 110.00   0.50    0.12    --  113.25-125.00   0.00  130
 33  ω     42.00  67.00   0.50    0.12    --  113.25-125.00 -30.00   50
 34  ω     84.00 110.00   0.50    0.12    --  113.25-125.00 -30.00   52
 35  ω     86.00 111.00   0.50    0.12    --  113.25-125.00 -90.00   50
 36  ω     52.00 107.00   0.50    0.12    --  113.25-125.00-150.00  110
 37  ω     51.00 109.00   0.50    0.12    --  113.25-125.00-180.00  116
 38  ω     62.00  88.00   0.50    0.05    --   47.77-125.00-180.00   52
 39  ω     79.00 105.00   0.50    0.12    --  113.25 -95.00-180.00   52
 40  ω     45.00  93.00   0.50    0.12    --  113.25 -95.00-150.00   96
 41  ω     35.00  94.00   0.50    0.05    --   47.77-125.00 -30.00  118
 42  ω     45.00 107.00   0.50    0.12    --  113.25-104.00 110.54  124
 43  ω     63.00  89.00   0.50    0.12    --  113.25-108.00  -0.57   52
 44  ω     64.00  94.00   0.50    0.12    --  113.25 -95.00 -90.00   60
 45  ω     43.00  90.00   0.50    0.12    --  113.25 -77.00-150.00   94
 46  ω     43.00  68.00   0.50    0.12    --  113.25 -61.00-150.00   50
 47  ω     42.00  91.00   0.50    0.12    --  113.25 -77.00 -90.00   98
 48  ω     43.00  68.00   0.50    0.12    --  113.25 -61.00 -90.00   50
 49  ω     50.00  85.00   0.50    0.12    --  113.25 -77.00  60.00   70
 50  ω     42.00  67.00   0.50    0.12    --  113.25 -61.00  90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0856027000
_diffrn_orient_matrix_UB_12      0.0723405000
_diffrn_orient_matrix_UB_13      -0.0804163000
_diffrn_orient_matrix_UB_21      0.0636886000
_diffrn_orient_matrix_UB_22      0.1567916000
_diffrn_orient_matrix_UB_23      -0.0071239000
_diffrn_orient_matrix_UB_31      0.1488294000
_diffrn_orient_matrix_UB_32      -0.0137772000
_diffrn_orient_matrix_UB_33      -0.0888688000
_diffrn_oxdiff_digest_frames     
;
0132248c46386eb3029e463f7ef6a1115204102a42a
;
_diffrn_oxdiff_digest_hkl        
;
01555f63190e4857330c8c4486ef0a1ec71366
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4224
_reflns_number_total             4450
_reflns_odcompleteness_completeness 99.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.567
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.442
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4450
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0829
_refine_ls_restrained_S_all      1.128
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1494P)²+2.2142P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2175
_refine_ls_wR_factor_ref         0.2197
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H3(0.075) H5(0.065) H7(0.062) H10(0.066) H6(0.063) H3A(0.065)
 H12(0.073) H11(0.08) H13(0.066) H14A(0.091) H14B(0.091) H14C(0.091)
 Fixed X: O10(0.5) H3(1.036632) H5(0.517096) H7(0.731182) H10(0.949)
 H6(0.623672) H3A(0.664051) H12(1.218237) H11(1.174006) H13(1.127788)
 H14A(0.461543) H14B(0.342845) H14C(0.325488)
 Fixed Y: O10(0.5) H3(-0.083818) H5(0.726253) H7(0.418916) H10(0.123049)
 H6(0.528792) H3A(1.008752) H12(0.144765) H11(-0.081321) H13(0.365828)
 H14A(0.949789) H14B(1.065909) H14C(0.892077)
 Fixed Z: O10(1) H3(0.800341) H5(0.309421) H7(0.540894) H10(0.709134)
 H6(0.403621) H3A(0.444643) H12(0.942127) H11(0.911541) H13(0.853857)
 H14A(0.208531) H14B(0.254524) H14C(0.318187)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo2 Mo 0.48225(8) 0.58200(8) 0.83005(5) 0.0495(2) Uani 1 1 d . . . . .
Mo4 Mo 0.23671(8) 0.40790(8) 1.06068(5) 0.0496(2) Uani 1 1 d . . . . .
Mo3 Mo 0.41842(8) 0.72976(8) 1.02779(5) 0.0507(2) Uani 1 1 d . . . . .
Mo1 Mo 0.94395(8) 0.72174(8) 0.62576(5) 0.0516(2) Uani 1 1 d . . . . .
O10 O 0.500000 0.500000 1.000000 0.0494(17) Uani 1 2 d S T P . .
O12 O 0.2195(7) 0.6105(7) 1.0691(5) 0.0512(13) Uani 1 1 d . . . . .
O14 O 0.4509(7) 0.6337(7) 1.1535(5) 0.0510(12) Uani 1 1 d . . . . .
O7 O 0.4084(7) 0.7429(7) 0.8818(5) 0.0528(13) Uani 1 1 d . . . . .
O8 O 0.2756(7) 0.4740(7) 0.9162(5) 0.0532(13) Uani 1 1 d . . . . .
O6 O 0.6999(7) 0.6300(7) 0.8067(5) 0.0522(13) Uani 1 1 d . . . . .
O2 O 1.0157(8) 0.5359(7) 0.7124(5) 0.0545(13) Uani 1 1 d . . . . .
O9 O 0.4628(8) 0.6215(8) 0.7097(5) 0.0577(14) Uani 1 1 d . . . . .
O15 O 0.6425(7) 0.7670(7) 0.9587(5) 0.0530(13) Uani 1 1 d . . . . .
O3 O 1.1093(9) 0.7627(8) 0.5190(6) 0.0640(16) Uani 1 1 d . . . . .
O13 O 0.3503(8) 0.8992(8) 1.0395(6) 0.0621(15) Uani 1 1 d . . . . .
O5 O 0.5075(8) 1.0044(8) 0.3246(5) 0.0597(14) Uani 1 1 d . . . . .
O4 O 0.9574(8) 0.8397(7) 0.6987(5) 0.0564(13) Uani 1 1 d . . . . .
O11 O 0.0489(8) 0.3352(7) 1.1021(5) 0.0550(13) Uani 1 1 d . . . . .
O1 O 0.7828(8) 0.8136(8) 0.5655(5) 0.0584(14) Uani 1 1 d . . . . .
N2 N 0.8741(9) 0.3817(9) 0.6622(6) 0.0532(15) Uani 1 1 d . . . . .
N1 N 0.8388(9) 0.5209(9) 0.6077(6) 0.0530(15) Uani 1 1 d . . . . .
N3 N 1.0552(11) 0.0032(10) 0.8099(7) 0.0624(18) Uani 1 1 d . . . . .
H3 H 1.036632 -0.083818 0.800341 0.075 Uiso 1 1 calc R . . . .
C8 C 0.9678(10) 0.4014(10) 0.7128(7) 0.0499(17) Uani 1 1 d . . . . .
C9 C 1.0251(10) 0.2667(10) 0.7731(7) 0.0531(18) Uani 1 1 d . . . . .
C5 C 0.5666(11) 0.7415(11) 0.3575(7) 0.0540(18) Uani 1 1 d . . . . .
H5 H 0.517096 0.726253 0.309421 0.065 Uiso 1 1 calc R . . . .
C7 C 0.7580(10) 0.5148(10) 0.5455(7) 0.0514(17) Uani 1 1 d . . . . .
H7 H 0.731182 0.418916 0.540894 0.062 Uiso 1 1 calc R . . . .
C10 C 1.0024(11) 0.1293(11) 0.7574(7) 0.0548(18) Uani 1 1 d . . . . .
H10 H 0.949000 0.123049 0.709134 0.066 Uiso 1 1 calc R . . . .
C4 C 0.5757(10) 0.8844(11) 0.3735(7) 0.0536(18) Uani 1 1 d . . . . .
C1 C 0.7072(10) 0.6453(10) 0.4835(7) 0.0521(17) Uani 1 1 d . . . . .
C6 C 0.6307(10) 0.6260(10) 0.4129(7) 0.0523(17) Uani 1 1 d . . . . .
H6 H 0.623672 0.528792 0.403621 0.063 Uiso 1 1 calc R . . . .
C3 C 0.6534(11) 0.9099(10) 0.4388(7) 0.0539(18) Uani 1 1 d . . . . .
H3A H 0.664051 1.008752 0.444643 0.065 Uiso 1 1 calc R . . . .
C12 C 1.1627(11) 0.1416(13) 0.8944(7) 0.061(2) Uani 1 1 d . . . . .
H12 H 1.218237 0.144765 0.942127 0.073 Uiso 1 1 calc R . . . .
C2 C 0.7170(10) 0.7904(10) 0.4966(6) 0.0484(16) Uani 1 1 d . . . . .
C11 C 1.1358(13) 0.0083(13) 0.8767(8) 0.067(2) Uani 1 1 d . . . . .
H11 H 1.174006 -0.081321 0.911541 0.080 Uiso 1 1 calc R . . . .
C13 C 1.1084(11) 0.2725(11) 0.8424(7) 0.0548(18) Uani 1 1 d . . . . .
H13 H 1.127788 0.365828 0.853857 0.066 Uiso 1 1 calc R . . . .
C14 C 0.4010(12) 0.9758(12) 0.2724(8) 0.061(2) Uani 1 1 d . . . . .
H14A H 0.461543 0.949789 0.208531 0.091 Uiso 1 1 calc GR . . . .
H14B H 0.342845 1.065909 0.254524 0.091 Uiso 1 1 calc GR . . . .
H14C H 0.325488 0.892077 0.318187 0.091 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo2 O10 2.3487(7) . ?
Mo2 O14 2.036(6) 2_667 ?
Mo2 O7 1.844(6) . ?
Mo2 O8 1.978(6) . ?
Mo2 O6 1.899(6) . ?
Mo2 O9 1.687(7) . ?
Mo4 O10 2.3244(7) . ?
Mo4 O12 1.908(6) . ?
Mo4 O8 1.874(6) . ?
Mo4 O6 2.041(6) 2_667 ?
Mo4 O15 1.945(6) 2_667 ?
Mo4 O11 1.680(6) . ?
Mo3 O10 2.3174(7) . ?
Mo3 O12 1.952(6) . ?
Mo3 O14 1.850(6) . ?
Mo3 O7 2.046(6) . ?
Mo3 O15 1.917(6) . ?
Mo3 O13 1.693(7) . ?
Mo1 O2 2.026(7) . ?
Mo1 O3 1.706(7) . ?
Mo1 O4 1.715(6) . ?
Mo1 O1 1.934(6) . ?
Mo1 N1 2.212(8) . ?
O2 C8 1.326(11) . ?
O5 C4 1.365(11) . ?
O5 C14 1.428(12) . ?
O1 C2 1.335(11) . ?
N2 N1 1.389(11) . ?
N2 C8 1.290(12) . ?
N1 C7 1.299(12) . ?
N3 H3 0.8800 . ?
N3 C10 1.353(13) . ?
N3 C11 1.351(15) . ?
C8 C9 1.475(13) . ?
C9 C10 1.379(13) . ?
C9 C13 1.401(13) . ?
C5 H5 0.9500 . ?
C5 C4 1.409(13) . ?
C5 C6 1.358(13) . ?
C7 H7 0.9500 . ?
C7 C1 1.431(13) . ?
C10 H10 0.9500 . ?
C4 C3 1.371(14) . ?
C1 C6 1.409(12) . ?
C1 C2 1.413(12) . ?
C6 H6 0.9500 . ?
C3 H3A 0.9500 . ?
C3 C2 1.396(13) . ?
C12 H12 0.9500 . ?
C12 C11 1.364(17) . ?
C12 C13 1.388(14) . ?
C11 H11 0.9500 . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O14 Mo2 O10 75.00(17) 2_667 . ?
O7 Mo2 O10 78.14(19) . . ?
O7 Mo2 O14 152.6(3) . 2_667 ?
O7 Mo2 O8 87.5(3) . . ?
O7 Mo2 O6 94.9(3) . . ?
O8 Mo2 O10 74.82(18) . . ?
O8 Mo2 O14 80.5(3) . 2_667 ?
O6 Mo2 O10 78.56(19) . . ?
O6 Mo2 O14 84.9(3) . 2_667 ?
O6 Mo2 O8 152.2(3) . . ?
O9 Mo2 O10 173.8(2) . . ?
O9 Mo2 O14 99.8(3) . 2_667 ?
O9 Mo2 O7 106.7(3) . . ?
O9 Mo2 O8 101.1(3) . . ?
O9 Mo2 O6 104.7(3) . . ?
O12 Mo4 O10 76.98(19) . . ?
O12 Mo4 O6 84.4(3) . 2_667 ?
O12 Mo4 O15 152.6(3) . 2_667 ?
O8 Mo4 O10 77.29(19) . . ?
O8 Mo4 O12 90.5(3) . . ?
O8 Mo4 O6 153.8(3) . 2_667 ?
O8 Mo4 O15 88.7(3) . 2_667 ?
O6 Mo4 O10 76.51(17) 2_667 . ?
O15 Mo4 O10 76.08(19) 2_667 . ?
O15 Mo4 O6 84.3(3) 2_667 2_667 ?
O11 Mo4 O10 177.5(2) . . ?
O11 Mo4 O12 105.4(3) . . ?
O11 Mo4 O8 101.8(3) . . ?
O11 Mo4 O6 104.4(3) . 2_667 ?
O11 Mo4 O15 101.6(3) . 2_667 ?
O12 Mo3 O10 76.34(18) . . ?
O12 Mo3 O7 82.0(3) . . ?
O14 Mo3 O10 79.20(19) . . ?
O14 Mo3 O12 90.5(3) . . ?
O14 Mo3 O7 154.4(3) . . ?
O14 Mo3 O15 91.8(3) . . ?
O7 Mo3 O10 75.23(18) . . ?
O15 Mo3 O10 76.75(18) . . ?
O15 Mo3 O12 152.0(3) . . ?
O15 Mo3 O7 83.9(3) . . ?
O13 Mo3 O10 174.7(3) . . ?
O13 Mo3 O12 101.2(3) . . ?
O13 Mo3 O14 105.7(3) . . ?
O13 Mo3 O7 99.8(3) . . ?
O13 Mo3 O15 105.0(3) . . ?
O2 Mo1 N1 71.5(3) . . ?
O3 Mo1 O2 99.0(3) . . ?
O3 Mo1 O4 106.3(3) . . ?
O3 Mo1 O1 101.1(3) . . ?
O3 Mo1 N1 101.4(3) . . ?
O4 Mo1 O2 96.9(3) . . ?
O4 Mo1 O1 101.2(3) . . ?
O4 Mo1 N1 151.3(3) . . ?
O1 Mo1 O2 147.9(3) . . ?
O1 Mo1 N1 80.0(3) . . ?
Mo2 O10 Mo2 180.0 . 2_667 ?
Mo4 O10 Mo2 89.74(2) . . ?
Mo4 O10 Mo2 89.74(2) 2_667 2_667 ?
Mo4 O10 Mo2 90.26(2) . 2_667 ?
Mo4 O10 Mo2 90.26(2) 2_667 . ?
Mo4 O10 Mo4 180.0 . 2_667 ?
Mo3 O10 Mo2 90.16(2) . . ?
Mo3 O10 Mo2 89.84(2) 2_667 . ?
Mo3 O10 Mo2 90.16(2) 2_667 2_667 ?
Mo3 O10 Mo2 89.84(2) . 2_667 ?
Mo3 O10 Mo4 89.94(2) 2_667 . ?
Mo3 O10 Mo4 89.94(2) . 2_667 ?
Mo3 O10 Mo4 90.06(2) . . ?
Mo3 O10 Mo4 90.06(2) 2_667 2_667 ?
Mo3 O10 Mo3 180.0 2_667 . ?
Mo4 O12 Mo3 116.6(3) . . ?
Mo3 O14 Mo2 115.9(3) . 2_667 ?
Mo2 O7 Mo3 116.2(3) . . ?
Mo4 O8 Mo2 117.7(3) . . ?
Mo2 O6 Mo4 114.4(3) . 2_667 ?
C8 O2 Mo1 119.1(6) . . ?
Mo3 O15 Mo4 116.3(3) . 2_667 ?
C4 O5 C14 117.8(8) . . ?
C2 O1 Mo1 136.0(6) . . ?
C8 N2 N1 109.0(7) . . ?
N2 N1 Mo1 117.0(5) . . ?
C7 N1 Mo1 128.4(6) . . ?
C7 N1 N2 114.4(7) . . ?
C10 N3 H3 119.3 . . ?
C11 N3 H3 119.3 . . ?
C11 N3 C10 121.3(9) . . ?
O2 C8 C9 118.8(8) . . ?
N2 C8 O2 123.4(8) . . ?
N2 C8 C9 117.8(8) . . ?
C10 C9 C8 118.9(8) . . ?
C10 C9 C13 118.1(9) . . ?
C13 C9 C8 123.0(8) . . ?
C4 C5 H5 121.0 . . ?
C6 C5 H5 121.0 . . ?
C6 C5 C4 118.0(9) . . ?
N1 C7 H7 118.3 . . ?
N1 C7 C1 123.3(8) . . ?
C1 C7 H7 118.3 . . ?
N3 C10 C9 120.8(9) . . ?
N3 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
O5 C4 C5 121.5(8) . . ?
O5 C4 C3 116.7(8) . . ?
C3 C4 C5 121.7(9) . . ?
C6 C1 C7 118.4(8) . . ?
C6 C1 C2 118.3(8) . . ?
C2 C1 C7 123.0(8) . . ?
C5 C6 C1 122.4(9) . . ?
C5 C6 H6 118.8 . . ?
C1 C6 H6 118.8 . . ?
C4 C3 H3A 120.1 . . ?
C4 C3 C2 119.9(9) . . ?
C2 C3 H3A 120.1 . . ?
C11 C12 H12 120.2 . . ?
C11 C12 C13 119.7(9) . . ?
C13 C12 H12 120.2 . . ?
O1 C2 C1 120.7(8) . . ?
O1 C2 C3 119.7(8) . . ?
C3 C2 C1 119.5(8) . . ?
N3 C11 C12 120.2(10) . . ?
N3 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C9 C13 H13 120.1 . . ?
C12 C13 C9 119.9(9) . . ?
C12 C13 H13 120.1 . . ?
O5 C14 H14A 109.5 . . ?
O5 C14 H14B 109.5 . . ?
O5 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O2 C8 N2 -1.6(11) . . . . ?
Mo1 O2 C8 C9 177.9(6) . . . . ?
Mo1 O1 C2 C1 28.2(13) . . . . ?
Mo1 O1 C2 C3 -153.4(7) . . . . ?
Mo1 N1 C7 C1 -7.3(13) . . . . ?
O10 Mo2 O7 Mo3 4.7(3) . . . . ?
O10 Mo2 O6 Mo4 -4.9(2) . . . 2_667 ?
O10 Mo4 O8 Mo2 -6.0(3) . . . . ?
O10 Mo3 O14 Mo2 -2.3(2) . . . 2_667 ?
O12 Mo4 O8 Mo2 70.5(4) . . . . ?
O12 Mo3 O14 Mo2 73.7(3) . . . 2_667 ?
O14 Mo2 O7 Mo3 16.1(8) 2_667 . . . ?
O14 Mo2 O6 Mo4 -80.6(3) 2_667 . . 2_667 ?
O7 Mo2 O6 Mo4 71.9(4) . . . 2_667 ?
O7 Mo3 O14 Mo2 1.3(8) . . . 2_667 ?
O8 Mo2 O7 Mo3 79.7(3) . . . . ?
O8 Mo2 O6 Mo4 -22.1(7) . . . 2_667 ?
O6 Mo2 O7 Mo3 -72.5(4) . . . . ?
O6 Mo4 O8 Mo2 -7.8(8) 2_667 . . . ?
O2 C8 C9 C10 -167.2(8) . . . . ?
O2 C8 C9 C13 9.8(13) . . . . ?
O9 Mo2 O7 Mo3 -179.4(3) . . . . ?
O9 Mo2 O6 Mo4 -179.4(3) . . . 2_667 ?
O15 Mo4 O8 Mo2 -82.1(4) 2_667 . . . ?
O15 Mo3 O14 Mo2 -78.4(3) . . . 2_667 ?
O13 Mo3 O14 Mo2 175.5(3) . . . 2_667 ?
O5 C4 C3 C2 175.8(8) . . . . ?
O11 Mo4 O8 Mo2 176.3(3) . . . . ?
N2 N1 C7 C1 179.0(8) . . . . ?
N2 C8 C9 C10 12.3(12) . . . . ?
N2 C8 C9 C13 -170.7(8) . . . . ?
N1 N2 C8 O2 1.7(11) . . . . ?
N1 N2 C8 C9 -177.7(7) . . . . ?
N1 C7 C1 C6 175.2(8) . . . . ?
N1 C7 C1 C2 -10.8(14) . . . . ?
C8 N2 N1 Mo1 -1.1(8) . . . . ?
C8 N2 N1 C7 173.4(8) . . . . ?
C8 C9 C10 N3 179.0(8) . . . . ?
C8 C9 C13 C12 -178.2(8) . . . . ?
C5 C4 C3 C2 -4.3(14) . . . . ?
C7 C1 C6 C5 174.2(8) . . . . ?
C7 C1 C2 O1 3.4(13) . . . . ?
C7 C1 C2 C3 -174.9(8) . . . . ?
C10 N3 C11 C12 1.5(15) . . . . ?
C10 C9 C13 C12 -1.2(13) . . . . ?
C4 C5 C6 C1 -1.1(13) . . . . ?
C4 C3 C2 O1 -175.3(8) . . . . ?
C4 C3 C2 C1 3.0(13) . . . . ?
C6 C5 C4 O5 -176.9(8) . . . . ?
C6 C5 C4 C3 3.3(13) . . . . ?
C6 C1 C2 O1 177.4(8) . . . . ?
C6 C1 C2 C3 -0.9(13) . . . . ?
C2 C1 C6 C5 0.0(13) . . . . ?
C11 N3 C10 C9 -2.1(14) . . . . ?
C11 C12 C13 C9 0.7(14) . . . . ?
C13 C9 C10 N3 1.9(13) . . . . ?
C13 C12 C11 N3 -0.8(15) . . . . ?
C14 O5 C4 C5 11.8(12) . . . . ?
C14 O5 C4 C3 -168.3(8) . . . . ?

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.279
_oxdiff_exptl_absorpt_empirical_full_min 0.353
# start Validation Reply Form
_vrf_PLAT430_exp_1871            
;
PROBLEM: Short Inter D...A Contact  O4       ..O6       .       2.80 Ang.  
RESPONSE: cis-MoO2 moiety is slightly skewed leading to closer than 
expected distances between neighboring oxygen atoms. 
However, no indications of errors in modelling the 
cis-MoO2 moiety were observed.
;
_vrf_PLAT971_exp_1871            
;
PROBLEM: Check Calcd Resid. Dens.  0.87Ang From Mo2             2.55 eA-3  
RESPONSE: Artifact due to insufficient data quality.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1H
_database_code_depnum_ccdc_archive 'CCDC 2335831'
loop_
_audit_author_name
_audit_author_address
'Mirta Rubcic'
;University of Zagreb
Croatia
;
_audit_update_record             
;
2024-02-27 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2021-03-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
(u6-oxo)-tetradecakis(u2-oxo)-octaoxo-bis(N-(2-oxy-3-(methoxy)benzylidene)nicotinylhydrazonato)-octa-molybdenum
_chemical_formula_moiety         'C28 H24 Mo8 N6 O29'
_chemical_formula_sum            'C28 H24 Mo8 N6 O29'
_chemical_formula_weight         1676.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         Mo
_chemical_oxdiff_usercomment     'zuta iglica 3py4OHsal'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
# end Validation Reply Form
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0670(6)
_cell_length_b                   10.0808(6)
_cell_length_c                   11.2764(7)
_cell_angle_alpha                90.460(5)
_cell_angle_beta                 92.740(5)
_cell_angle_gamma                108.443(5)
_cell_volume                     1084.03(12)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2821
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.4940
_cell_measurement_theta_min      4.2710
_shelx_estimated_absorpt_T_max   0.835
_shelx_estimated_absorpt_T_min   0.615
_exptl_absorpt_coefficient_mu    2.343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.567
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             802
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_unetI/netI     0.1572
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15537
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.002
_diffrn_reflns_theta_min         4.104
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -43.00   -1.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  -77.0000  -90.0000 42

#__ type_ start__ end____ width___ exp.time_
  2 omega  -44.00    1.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  -77.0000 -180.0000 45

#__ type_ start__ end____ width___ exp.time_
  3 omega    7.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   77.0000   30.0000 82

#__ type_ start__ end____ width___ exp.time_
  4 omega   -3.00   72.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   77.0000 -150.0000 75

#__ type_ start__ end____ width___ exp.time_
  5 omega   -6.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  -99.0000  120.0000 65

#__ type_ start__ end____ width___ exp.time_
  6 omega   35.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432  179.0000  120.0000 49

#__ type_ start__ end____ width___ exp.time_
  7 omega    1.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.3432   77.0000  -60.0000 86

#__ type_ start__ end____ width___ exp.time_
  8 omega  -75.00  -49.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4994  179.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
  9 omega  -17.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4994   19.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
 10 omega  -48.00  -22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4994   19.0000    0.0000 26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0625542000
_diffrn_orient_matrix_UB_12      0.0577020000
_diffrn_orient_matrix_UB_13      0.0061131000
_diffrn_orient_matrix_UB_21      0.0395283000
_diffrn_orient_matrix_UB_22      -0.0465718000
_diffrn_orient_matrix_UB_23      0.0084297000
_diffrn_orient_matrix_UB_31      0.0075162000
_diffrn_orient_matrix_UB_32      -0.0024789000
_diffrn_orient_matrix_UB_33      -0.0621255000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4159
_reflns_number_total             7115
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.173
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.242
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         7115
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1312
_refine_ls_R_factor_gt           0.0598
_refine_ls_restrained_S_all      0.934
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0090P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0737
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 N3-H3
 0.82 with sigma of 0.02
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C5(H5), C11(H11), C13(H13), C4(H4), C10(H10), C12(H12)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.75383(5) 0.08534(5) 0.26857(4) 0.01353(12) Uani 1 1 d . . . . .
Mo4 Mo 0.29190(5) 0.33397(5) 0.05290(4) 0.01397(12) Uani 1 1 d . . . . .
Mo2 Mo 0.62880(5) 0.38516(5) 0.10877(4) 0.01457(12) Uani 1 1 d . . . . .
Mo3 Mo 0.49674(5) 0.63433(5) 0.16658(4) 0.01500(12) Uani 1 1 d . . . . .
O11 O 0.500000 0.500000 0.000000 0.0134(12) Uani 1 2 d S T P . .
O9 O 0.5796(4) 0.5008(4) 0.2266(3) 0.0155(9) Uani 1 1 d . . . . .
O7 O 0.6093(4) 0.2999(3) -0.0431(3) 0.0163(9) Uani 1 1 d . . . . .
O14 O 0.3154(4) 0.4722(4) 0.1660(3) 0.0177(9) Uani 1 1 d . . . . .
O10 O 0.4279(4) 0.2678(3) 0.1226(3) 0.0147(9) Uani 1 1 d . . . . .
O12 O 0.6604(4) 0.7379(3) 0.1023(3) 0.0177(9) Uani 1 1 d . . . . .
O8 O 0.7680(4) 0.5401(4) 0.0615(3) 0.0165(9) Uani 1 1 d . . . . .
O1 O 0.9108(4) 0.2195(4) 0.3504(3) 0.0165(9) Uani 1 1 d . . . . .
O2 O 0.5499(4) 0.0261(3) 0.2150(3) 0.0148(9) Uani 1 1 d . . . . .
O6 O 0.7173(4) 0.2972(4) 0.1921(3) 0.0195(9) Uani 1 1 d . . . . .
O3 O 0.7580(4) -0.0617(4) 0.3384(3) 0.0200(9) Uani 1 1 d . . . . .
O4 O 0.8162(4) 0.0800(4) 0.1308(3) 0.0187(9) Uani 1 1 d . . . . .
O5 O 1.1754(4) 0.3055(4) 0.4234(3) 0.0221(10) Uani 1 1 d . . . . .
O15 O 0.1375(4) 0.2114(4) 0.0756(3) 0.0213(10) Uani 1 1 d . . . . .
O13 O 0.4817(4) 0.7230(4) 0.2889(3) 0.0224(10) Uani 1 1 d . . . . .
N1 N 0.6411(5) 0.1604(4) 0.4044(4) 0.0151(11) Uani 1 1 d . . . . .
N3 N 0.1271(5) -0.1034(5) 0.1093(4) 0.0181(11) Uani 1 1 d D . . . .
N2 N 0.4949(5) 0.1180(5) 0.3874(4) 0.0162(11) Uani 1 1 d . . . . .
C1 C 0.8378(6) 0.2938(5) 0.5335(5) 0.0131(12) Uani 1 1 d . . . . .
C7 C 0.6915(6) 0.2387(6) 0.4977(5) 0.0186(13) Uani 1 1 d . . . . .
H7 H 0.628319 0.260940 0.545346 0.022 Uiso 1 1 calc R . . . .
C2 C 0.9423(6) 0.2768(5) 0.4605(5) 0.0133(12) Uani 1 1 d . . . . .
C8 C 0.4604(6) 0.0497(5) 0.2882(5) 0.0140(12) Uani 1 1 d . . . . .
C6 C 0.8793(7) 0.3633(6) 0.6444(5) 0.0225(15) Uani 1 1 d . . . . .
H6 H 0.812131 0.377525 0.692342 0.027 Uiso 1 1 calc R . . . .
C5 C 1.0177(7) 0.4101(6) 0.6820(5) 0.0229(14) Uani 1 1 d . . . . .
H5 H 1.043917 0.455192 0.755745 0.027 Uiso 1 1 calc R . . . .
C11 C 0.0286(6) -0.0992(6) 0.1843(5) 0.0187(13) Uani 1 1 d . . . . .
H11 H -0.065947 -0.131961 0.160016 0.022 Uiso 1 1 calc R . . . .
C13 C 0.2077(6) 0.0016(5) 0.3308(5) 0.0153(12) Uani 1 1 d . . . . .
H13 H 0.235084 0.039242 0.406982 0.018 Uiso 1 1 calc R . . . .
C4 C 1.1184(6) 0.3912(5) 0.6117(5) 0.0191(13) Uani 1 1 d . . . . .
H4 H 1.211957 0.422682 0.639140 0.023 Uiso 1 1 calc R . . . .
C10 C 0.2640(6) -0.0593(5) 0.1404(5) 0.0159(13) Uani 1 1 d . . . . .
H10 H 0.328743 -0.065193 0.086125 0.019 Uiso 1 1 calc R . . . .
C12 C 0.0695(6) -0.0464(6) 0.2964(5) 0.0187(13) Uani 1 1 d . . . . .
H12 H 0.002622 -0.043142 0.349458 0.022 Uiso 1 1 calc R . . . .
C3 C 1.0833(6) 0.3264(5) 0.5013(5) 0.0180(13) Uani 1 1 d . . . . .
C14 C 1.3201(6) 0.3626(6) 0.4572(5) 0.0260(15) Uani 1 1 d . . . . .
H14A H 1.374533 0.341246 0.396620 0.039 Uiso 1 1 calc GR . . . .
H14B H 1.339402 0.323032 0.530653 0.039 Uiso 1 1 calc GR . . . .
H14C H 1.344387 0.462263 0.467313 0.039 Uiso 1 1 calc GR . . . .
C9 C 0.3092(6) -0.0050(5) 0.2531(5) 0.0126(12) Uani 1 1 d . . . . .
H3 H 0.111(6) -0.129(5) 0.041(2) 0.015 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O1 1.915(4) . ?
Mo1 O2 2.009(4) . ?
Mo1 O6 2.436(4) . ?
Mo1 O3 1.695(4) . ?
Mo1 O4 1.710(3) . ?
Mo1 N1 2.213(4) . ?
Mo4 O11 2.3373(5) . ?
Mo4 O14 1.833(3) . ?
Mo4 O10 1.849(4) . ?
Mo4 O12 2.024(3) 2_665 ?
Mo4 O8 2.019(4) 2_665 ?
Mo4 O15 1.684(4) . ?
Mo2 O11 2.3122(5) . ?
Mo2 O9 1.943(3) . ?
Mo2 O7 1.884(4) . ?
Mo2 O10 2.008(3) . ?
Mo2 O8 1.841(3) . ?
Mo2 O6 1.702(4) . ?
Mo3 O11 2.3144(5) . ?
Mo3 O9 1.907(4) . ?
Mo3 O7 1.959(4) 2_665 ?
Mo3 O14 2.028(4) . ?
Mo3 O12 1.835(4) . ?
Mo3 O13 1.676(3) . ?
O1 C2 1.346(6) . ?
O2 C8 1.324(6) . ?
O5 C3 1.369(6) . ?
O5 C14 1.418(6) . ?
N1 N2 1.400(6) . ?
N1 C7 1.292(7) . ?
N3 C11 1.344(7) . ?
N3 C10 1.336(7) . ?
N2 C8 1.283(6) . ?
C1 C7 1.436(7) . ?
C1 C2 1.417(7) . ?
C1 C6 1.407(7) . ?
C2 C3 1.400(8) . ?
C8 C9 1.478(7) . ?
C6 C5 1.367(8) . ?
C5 C4 1.375(8) . ?
C11 C12 1.360(7) . ?
C13 C12 1.357(7) . ?
C13 C9 1.393(7) . ?
C4 C3 1.379(7) . ?
C10 C9 1.377(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mo1 O2 148.64(15) . . ?
O1 Mo1 O6 81.64(15) . . ?
O1 Mo1 N1 81.01(16) . . ?
O2 Mo1 O6 75.46(13) . . ?
O2 Mo1 N1 72.20(16) . . ?
O3 Mo1 O1 99.72(17) . . ?
O3 Mo1 O2 99.42(16) . . ?
O3 Mo1 O6 170.13(15) . . ?
O3 Mo1 O4 107.27(17) . . ?
O3 Mo1 N1 96.93(16) . . ?
O4 Mo1 O1 101.41(16) . . ?
O4 Mo1 O2 96.30(16) . . ?
O4 Mo1 O6 81.88(15) . . ?
O4 Mo1 N1 154.75(18) . . ?
N1 Mo1 O6 73.55(15) . . ?
O14 Mo4 O11 78.05(11) . . ?
O14 Mo4 O10 94.23(16) . . ?
O14 Mo4 O12 151.75(14) . 2_665 ?
O14 Mo4 O8 86.84(16) . 2_665 ?
O10 Mo4 O11 77.35(10) . . ?
O10 Mo4 O12 85.82(16) . 2_665 ?
O10 Mo4 O8 151.18(15) . 2_665 ?
O12 Mo4 O11 74.41(10) 2_665 . ?
O8 Mo4 O11 74.71(10) 2_665 . ?
O8 Mo4 O12 80.06(15) 2_665 2_665 ?
O15 Mo4 O11 173.95(14) . . ?
O15 Mo4 O14 106.65(17) . . ?
O15 Mo4 O10 105.76(18) . . ?
O15 Mo4 O12 100.46(16) . 2_665 ?
O15 Mo4 O8 101.46(17) . 2_665 ?
O9 Mo2 O11 76.18(11) . . ?
O9 Mo2 O10 82.14(14) . . ?
O7 Mo2 O11 77.15(11) . . ?
O7 Mo2 O9 152.53(16) . . ?
O7 Mo2 O10 84.80(15) . . ?
O10 Mo2 O11 75.08(11) . . ?
O8 Mo2 O11 78.60(12) . . ?
O8 Mo2 O9 89.47(15) . . ?
O8 Mo2 O7 91.63(16) . . ?
O8 Mo2 O10 153.58(16) . . ?
O6 Mo2 O11 177.52(13) . . ?
O6 Mo2 O9 102.70(17) . . ?
O6 Mo2 O7 103.69(17) . . ?
O6 Mo2 O10 102.62(17) . . ?
O6 Mo2 O8 103.66(18) . . ?
O9 Mo3 O11 76.77(11) . . ?
O9 Mo3 O7 151.52(15) . 2_665 ?
O9 Mo3 O14 84.14(15) . . ?
O7 Mo3 O11 75.72(10) 2_665 . ?
O7 Mo3 O14 81.83(15) 2_665 . ?
O14 Mo3 O11 75.05(10) . . ?
O12 Mo3 O11 78.40(11) . . ?
O12 Mo3 O9 92.20(16) . . ?
O12 Mo3 O7 89.39(16) . 2_665 ?
O12 Mo3 O14 153.34(15) . . ?
O13 Mo3 O11 175.49(13) . . ?
O13 Mo3 O9 103.29(18) . . ?
O13 Mo3 O7 103.55(18) . 2_665 ?
O13 Mo3 O14 100.45(16) . . ?
O13 Mo3 O12 106.08(16) . . ?
Mo4 O11 Mo4 180.0 . 2_665 ?
Mo2 O11 Mo4 89.792(19) . 2_665 ?
Mo2 O11 Mo4 90.208(19) 2_665 2_665 ?
Mo2 O11 Mo4 89.791(19) 2_665 . ?
Mo2 O11 Mo4 90.209(19) . . ?
Mo2 O11 Mo2 180.0 2_665 . ?
Mo2 O11 Mo3 90.171(19) 2_665 . ?
Mo2 O11 Mo3 89.830(19) . . ?
Mo2 O11 Mo3 90.170(19) . 2_665 ?
Mo2 O11 Mo3 89.829(19) 2_665 2_665 ?
Mo3 O11 Mo4 90.114(17) . 2_665 ?
Mo3 O11 Mo4 89.886(18) . . ?
Mo3 O11 Mo4 89.886(18) 2_665 2_665 ?
Mo3 O11 Mo4 90.113(18) 2_665 . ?
Mo3 O11 Mo3 180.0 2_665 . ?
Mo3 O9 Mo2 116.09(18) . . ?
Mo2 O7 Mo3 116.96(17) . 2_665 ?
Mo4 O14 Mo3 116.56(17) . . ?
Mo4 O10 Mo2 117.21(17) . . ?
Mo3 O12 Mo4 117.01(17) . 2_665 ?
Mo2 O8 Mo4 116.41(19) . 2_665 ?
C2 O1 Mo1 136.8(3) . . ?
C8 O2 Mo1 118.1(4) . . ?
Mo2 O6 Mo1 153.3(2) . . ?
C3 O5 C14 116.7(5) . . ?
N2 N1 Mo1 116.0(3) . . ?
C7 N1 Mo1 129.0(4) . . ?
C7 N1 N2 115.1(4) . . ?
C10 N3 C11 122.8(5) . . ?
C8 N2 N1 108.4(4) . . ?
C2 C1 C7 121.4(5) . . ?
C6 C1 C7 119.8(5) . . ?
C6 C1 C2 118.8(6) . . ?
N1 C7 C1 124.9(5) . . ?
O1 C2 C1 121.9(5) . . ?
O1 C2 C3 118.6(5) . . ?
C3 C2 C1 119.5(5) . . ?
O2 C8 C9 118.0(5) . . ?
N2 C8 O2 124.9(5) . . ?
N2 C8 C9 117.1(5) . . ?
C5 C6 C1 120.4(5) . . ?
C6 C5 C4 120.6(6) . . ?
N3 C11 C12 118.9(6) . . ?
C12 C13 C9 120.7(6) . . ?
C5 C4 C3 121.2(6) . . ?
N3 C10 C9 119.8(5) . . ?
C13 C12 C11 120.1(5) . . ?
O5 C3 C2 114.6(5) . . ?
O5 C3 C4 125.8(6) . . ?
C4 C3 C2 119.6(5) . . ?
C13 C9 C8 121.4(5) . . ?
C10 C9 C8 120.9(5) . . ?
C10 C9 C13 117.6(5) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT910_exp_3786            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         14 Note  
RESPONSE: Low-angle reflections are shadowed by beam-stop, and not included
in integration.
;
_vrf_PLAT973_exp_3786            
;
PROBLEM: Check Calcd Positive Resid. Density on       Mo1       1.56 eA-3  
RESPONSE: Artifact due to insufficient data quality.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3H-2CH3CN
_database_code_depnum_ccdc_archive 'CCDC 2335832'
loop_
_audit_author_name
_audit_author_address
'Mirta Rubcic'
;University of Zagreb
Croatia
;
_audit_update_record             
;
2024-02-27 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-04-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Mo6 O19, 2(C14 H12 Mo N3 O5), 2(C2 H3 N)'
_chemical_formula_sum            'C32 H30 Mo8 N8 O29'
_chemical_formula_weight         1758.16
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Mo8 O25 C30 N8'
_chemical_oxdiff_usercomment     ' '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.02310(10)
_cell_length_b                   10.7273(3)
_cell_length_c                   12.9277(3)
_cell_angle_alpha                73.422(2)
_cell_angle_beta                 72.752(2)
_cell_angle_gamma                66.204(2)
_cell_volume                     1192.60(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    11444
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      77.3170
_cell_measurement_theta_min      3.6510
_shelx_estimated_absorpt_T_max   0.611
_shelx_estimated_absorpt_T_min   0.158
_exptl_absorpt_coefficient_mu    17.600
_exptl_absorpt_correction_T_max  0.696
_exptl_absorpt_correction_T_min  0.149
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.448
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             846
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -6 -6 0.0355
3 6 6 0.0355
6 0 0 0.0857
-6 0 0 0.0507
0 0 8 0.0153
0 0 -8 0.0153

_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.031
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.1102 -6.0861 -5.9887 -0.8444 -0.4589 -0.2765
3.1102 6.0861 5.9887 0.8444 0.4589 0.2765
5.8556 0.1910 -0.1693 -0.1998 -0.1152 0.9730
-5.8462 -0.1708 0.1892 0.2027 0.1168 -0.9723
-0.0388 -0.1833 7.8114 0.0234 0.9931 -0.1149
0.0388 0.1833 -7.8114 -0.0234 -0.9931 0.1149

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17780
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.711
_diffrn_reflns_theta_min         3.646
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    103.00 132.00   0.50    0.33    --  107.75  77.00 -60.00   58
  2  ω    137.00 162.00   0.50    0.33    --  107.75  77.00 -60.00   50
  3  ω    106.00 174.00   0.50    0.33    --  107.75  45.00-150.00  136
  4  ω     98.00 176.00   0.50    0.33    --  107.75  45.00 -60.00  156
  5  ω    105.00 146.00   0.50    0.33    --  107.75  15.00-150.00   82
  6  ω    110.00 178.00   0.50    0.33    --  107.75  45.00  30.00  136
  7  ω    120.00 174.00   0.50    0.33    --  107.75  45.00  60.00  108
  8  ω     95.00 123.00   0.50    0.33    --  107.75  30.00 120.00   56
  9  ω    128.00 154.00   0.50    0.33    --  107.75  30.00 120.00   52
 10  ω    -24.00  26.00   0.50    0.08    --  -47.03  19.00-120.00  100
 11  ω     -8.00  27.00   0.50    0.08    --  -47.03  19.00 -90.00   70
 12  ω    -44.00 -14.00   0.50    0.33    --  -86.25  45.00   0.00   60
 13  ω    -17.00   8.00   0.50    0.08    --  -47.03  19.00  30.00   50
 14  ω    -25.00  28.00   0.50    0.08    --  -47.03  19.00 150.00  106
 15  ω    100.00 154.00   0.50    0.33    --  107.75 121.00 128.00  108
 16  ω    136.00 161.00   0.50    0.33    --  107.75 125.00  60.00   50
 17  ω     95.00 121.00   0.50    0.33    --  107.75 125.00  60.00   52
 18  ω     94.00 119.00   0.50    0.33    --  107.75 155.00 -73.00   50
 19  ω     95.00 174.00   0.50    0.33    --  107.75 125.00 -30.00  158
 20  ω    -21.00  25.00   0.50    0.08    --   47.03 -19.00   0.00   92
 21  ω     37.00  89.00   0.50    0.33    --  107.75 -77.00 150.00  104
 22  ω     61.00  86.00   0.50    0.33    --  107.75 -77.00  90.00   50
 23  ω     37.00  64.00   0.50    0.33    --  107.75 -61.00 120.00   54
 24  ω     55.00 105.00   0.50    0.33    --  107.75 -77.00  30.00  100
 25  ω     35.00  71.00   0.50    0.33    --  107.75 -61.00  30.00   72
 26  ω     40.00  67.00   0.50    0.33    --  107.75 -61.00   0.00   54
 27  ω     37.00  69.00   0.50    0.33    --  107.75 -61.00 -60.00   64
 28  ω     35.00  64.00   0.50    0.33    --  107.75 -61.00-120.00   58
 29  ω     39.00  64.00   0.50    0.33    --  107.75 -61.00-150.00   50
 30  ω     71.00  96.00   0.50    0.33    --  107.75 -77.00 -90.00   50
 31  ω     37.00  71.00   0.50    0.33    --  107.75 -61.00  60.00   68
 32  ω     44.00  69.00   0.50    0.33    --  107.75 -61.00  90.00   50
 33  ω     76.00 102.00   0.50    0.33    --  107.75 -95.00 -60.00   52
 34  ω     81.00 107.00   0.50    0.33    --  107.75-125.00-120.00   52
 35  ω     74.00 133.00   0.50    0.33    --  107.75-155.00-112.00  118
 36  ω     58.00 113.00   0.50    0.08    --   47.03-155.00-112.00  110
 37  ω     64.00 112.00   0.50    0.33    --  107.75-125.00 -90.00   96
 38  ω     40.00 111.00   0.50    0.33    --  107.75-125.00 -60.00  142
 39  ω     37.00 112.00   0.50    0.33    --  107.75-125.00  30.00  150
 40  ω     83.00 109.00   0.50    0.33    --  107.75-125.00  90.00   52
 41  ω     80.00 108.00   0.50    0.33    --  107.75-125.00 150.00   56
 42  ω     86.00 111.00   0.50    0.33    --  107.75-125.00 120.00   50
 43  ω     35.00  67.00   0.50    0.33    --  107.75-125.00 150.00   64
 44  ω     40.00  93.00   0.50    0.08    --   47.03-121.00  45.00  106
 45  ω     72.00 109.00   0.50    0.33    --  107.75-121.00  45.00   74
 46  ω     58.00  84.00   0.50    0.33    --  107.75 -95.00  60.00   52
 47  ω     38.00  69.00   0.50    0.33    --  107.75 -95.00 -60.00   62
 48  ω     38.00  68.00   0.50    0.33    --  107.75-125.00-180.00   60
 49  ω     79.00 109.00   0.50    0.33    --  107.75-125.00-180.00   60
 50  ω   -125.00 -88.00   0.50    0.33    --  -86.25 -30.00 -90.00   74
 51  ω   -123.00 -98.00   0.50    0.33    --  -86.25-155.00-112.00   50
 52  ω    -95.00 -53.00   0.50    0.08    --  -47.03-155.00-112.00   84
 53  ω   -114.00 -79.00   0.50    0.33    --  -86.25-121.00  45.00   70
 54  ω   -107.00 -82.00   0.50    0.08    --  -47.03-125.00  60.00   50
 55  ω    -40.00 -14.00   0.50    0.08    --  -47.03 121.00 128.00   52
 56  ω    -56.00 -29.00   0.50    0.33    --  -86.25 121.00 128.00   54
 57  ω    -81.00 -55.00   0.50    0.08    --  -47.03 155.00 -73.00   52
 58  ω    -92.00 -67.00   0.50    0.33    --  -86.25 155.00 -73.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0389136000
_diffrn_orient_matrix_UB_12      0.1523517000
_diffrn_orient_matrix_UB_13      0.0063754000
_diffrn_orient_matrix_UB_21      -0.0146922000
_diffrn_orient_matrix_UB_22      -0.0411725000
_diffrn_orient_matrix_UB_23      0.1260953000
_diffrn_orient_matrix_UB_31      0.1665804000
_diffrn_orient_matrix_UB_32      -0.0254426000
_diffrn_orient_matrix_UB_33      -0.0144812000
_diffrn_oxdiff_digest_frames     
;
0140d9eb0e04fff2879d2bbf85e9a92cb80439634f0
;
_diffrn_oxdiff_digest_hkl        
;
013db9e7c0544c078e89abe526e7f38d8c5bc3
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4572
_reflns_number_total             4996
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.475
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       0.00047(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4996
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0360
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0604P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0968
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H3(0.022) H7(0.021) H10(0.022) H4(0.027) H6(0.025) H3A(0.026)
 H14A(0.036) H14B(0.036) H14C(0.036) H13(0.024) H11(0.026) H12(0.027)
 H16A(0.092) H16B(0.092) H16C(0.092)
 Fixed X: O11(0) H3(0.506666) H7(0.743632) H10(0.543561) H4(0.821504)
 H6(0.836937) H3A(0.702669) H14A(0.853293) H14B(0.993632) H14C(1.010493)
 H13(0.65012) H11(0.537928) H12(0.612386) H16A(0.134989) H16B(0.182689)
 H16C(0.087366)
 Fixed Y: O11(0.5) H3(0.252803) H7(-0.028288) H10(0.328639) H4(0.210967) H6(-
 0.085421) H3A(0.383256) H14A(0.023577) H14B(-0.118002) H14C(0.021655) H13(-
 0.066861) H11(0.032199) H12(-0.134297) H16A(0.462677) H16B(0.407933)
 H16C(0.33984)
 Fixed Z: O11(0.5) H3(0.776525) H7(0.229842) H10(0.594342) H4(-0.225097)
 H6(0.052113) H3A(-0.117414) H14A(-0.299413) H14B(-0.297794) H14C(-0.291541)
 H13(0.56187) H11(0.862593) H12(0.753399) H16A(1.013769) H16B(1.130884)
 H16C(1.100024)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo2 Mo 0.22651(3) 0.42845(3) 0.37736(2) 0.01558(11) Uani 1 1 d . . . . .
Mo3 Mo -0.11562(3) 0.62899(3) 0.35296(3) 0.01677(11) Uani 1 1 d . . . . .
Mo1 Mo 0.65053(3) 0.37500(3) 0.22849(3) 0.01632(11) Uani 1 1 d . . . . .
Mo4 Mo -0.04949(3) 0.31093(3) 0.49058(3) 0.01650(11) Uani 1 1 d . . . . .
O2 O 0.6099(3) 0.3148(3) 0.3943(2) 0.0179(5) Uani 1 1 d . . . . .
O11 O 0.000000 0.500000 0.500000 0.0137(7) Uani 1 2 d S T P . .
O8 O 0.2256(3) 0.5920(3) 0.3994(2) 0.0182(5) Uani 1 1 d . . . . .
O10 O 0.1283(3) 0.2943(3) 0.3877(2) 0.0192(5) Uani 1 1 d . . . . .
O15 O 0.0519(3) 0.2425(3) 0.6096(2) 0.0192(6) Uani 1 1 d . . . . .
O13 O -0.1543(3) 0.4625(3) 0.3849(2) 0.0186(6) Uani 1 1 d . . . . .
O9 O 0.0789(3) 0.5474(3) 0.2817(2) 0.0187(5) Uani 1 1 d . . . . .
O7 O 0.2760(3) 0.3273(3) 0.5109(2) 0.0206(6) Uani 1 1 d . . . . .
O1 O 0.6336(3) 0.3553(3) 0.0910(2) 0.0207(6) Uani 1 1 d . . . . .
O12 O -0.2085(3) 0.7291(3) 0.2511(3) 0.0232(6) Uani 1 1 d . . . . .
O14 O -0.0955(3) 0.1766(3) 0.4892(3) 0.0223(6) Uani 1 1 d . . . . .
O4 O 0.5504(3) 0.5478(3) 0.2284(3) 0.0248(6) Uani 1 1 d . . . . .
O5 O 0.9031(4) -0.0624(3) -0.1515(3) 0.0309(7) Uani 1 1 d . . . . .
N2 N 0.6590(4) 0.0898(3) 0.3790(3) 0.0182(6) Uani 1 1 d . . . . .
O6 O 0.3851(3) 0.3729(3) 0.2813(2) 0.0213(6) Uani 1 1 d . . . . .
N3 N 0.5352(3) 0.1909(4) 0.7348(3) 0.0181(6) Uani 1 1 d . . . . .
H3 H 0.506666 0.252803 0.776525 0.022 Uiso 1 1 calc R . . . .
N1 N 0.6793(3) 0.1511(3) 0.2680(3) 0.0163(6) Uani 1 1 d . . . . .
O3 O 0.8318(3) 0.3552(4) 0.2012(3) 0.0295(7) Uani 1 1 d . . . . .
C7 C 0.7249(4) 0.0677(4) 0.2003(3) 0.0176(7) Uani 1 1 d . . . . .
H7 H 0.743632 -0.028288 0.229842 0.021 Uiso 1 1 calc R . . . .
C1 C 0.7490(4) 0.1117(4) 0.0826(3) 0.0189(8) Uani 1 1 d . . . . .
C10 C 0.5572(4) 0.2338(4) 0.6254(3) 0.0185(7) Uani 1 1 d . . . . .
H10 H 0.543561 0.328639 0.594342 0.022 Uiso 1 1 calc R . . . .
C9 C 0.5999(4) 0.1394(4) 0.5581(3) 0.0152(7) Uani 1 1 d . . . . .
C8 C 0.6255(4) 0.1834(4) 0.4364(3) 0.0173(7) Uani 1 1 d . . . . .
C4 C 0.8011(5) 0.1855(5) -0.1469(3) 0.0224(8) Uani 1 1 d . . . . .
H4 H 0.821504 0.210967 -0.225097 0.027 Uiso 1 1 calc R . . . .
C6 C 0.8125(4) 0.0096(4) 0.0176(4) 0.0206(8) Uani 1 1 d . . . . .
H6 H 0.836937 -0.085421 0.052113 0.025 Uiso 1 1 calc R . . . .
C3 C 0.7318(4) 0.2883(4) -0.0825(3) 0.0218(8) Uani 1 1 d . . . . .
H3A H 0.702669 0.383256 -0.117414 0.026 Uiso 1 1 calc R . . . .
C14 C 0.9433(5) -0.0313(5) -0.2694(3) 0.0243(8) Uani 1 1 d . . . . .
H14A H 0.853293 0.023577 -0.299413 0.036 Uiso 1 1 calc GR . . . .
H14B H 0.993632 -0.118002 -0.297794 0.036 Uiso 1 1 calc GR . . . .
H14C H 1.010493 0.021655 -0.291541 0.036 Uiso 1 1 calc GR . . . .
C13 C 0.6206(4) -0.0001(4) 0.6068(4) 0.0199(8) Uani 1 1 d . . . . .
H13 H 0.650120 -0.066861 0.561870 0.024 Uiso 1 1 calc R . . . .
C5 C 0.8403(4) 0.0455(4) -0.0968(4) 0.0214(8) Uani 1 1 d . . . . .
C2 C 0.7052(4) 0.2536(4) 0.0314(3) 0.0186(7) Uani 1 1 d . . . . .
N4 N 0.4101(6) 0.2013(6) 0.9898(4) 0.0458(11) Uani 1 1 d . . . . .
C11 C 0.5543(4) 0.0581(4) 0.7845(4) 0.0214(8) Uani 1 1 d . . . . .
H11 H 0.537928 0.032199 0.862593 0.026 Uiso 1 1 calc R . . . .
C12 C 0.5980(4) -0.0399(4) 0.7200(4) 0.0226(8) Uani 1 1 d . . . . .
H12 H 0.612386 -0.134297 0.753399 0.027 Uiso 1 1 calc R . . . .
C15 C 0.3003(6) 0.2812(6) 1.0247(4) 0.0332(10) Uani 1 1 d . . . . .
C16 C 0.1658(7) 0.3807(8) 1.0710(7) 0.0612(18) Uani 1 1 d . . . . .
H16A H 0.134989 0.462677 1.013769 0.092 Uiso 1 1 calc GR . . . .
H16B H 0.182689 0.407933 1.130884 0.092 Uiso 1 1 calc GR . . . .
H16C H 0.087366 0.339840 1.100024 0.092 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo2 O11 2.3261(3) . ?
Mo2 O8 1.852(3) . ?
Mo2 O10 2.003(3) . ?
Mo2 O9 2.002(3) . ?
Mo2 O7 1.846(3) . ?
Mo2 O6 1.707(3) . ?
Mo3 O11 2.3200(3) . ?
Mo3 O15 1.954(3) 2_566 ?
Mo3 O13 1.885(3) . ?
Mo3 O9 1.853(3) . ?
Mo3 O7 2.022(3) 2_566 ?
Mo3 O12 1.693(3) . ?
Mo1 O2 2.020(3) . ?
Mo1 O1 1.912(3) . ?
Mo1 O4 1.715(3) . ?
Mo1 N1 2.223(3) . ?
Mo1 O3 1.680(3) . ?
Mo4 O11 2.3158(3) . ?
Mo4 O8 2.024(3) 2_566 ?
Mo4 O10 1.857(3) . ?
Mo4 O15 1.902(3) . ?
Mo4 O13 1.954(3) . ?
Mo4 O14 1.687(3) . ?
O2 C8 1.320(5) . ?
O1 C2 1.348(5) . ?
O5 C14 1.432(5) . ?
O5 C5 1.361(5) . ?
N2 N1 1.389(5) . ?
N2 C8 1.294(5) . ?
N3 H3 0.8800 . ?
N3 C10 1.336(5) . ?
N3 C11 1.345(6) . ?
N1 C7 1.286(5) . ?
C7 H7 0.9500 . ?
C7 C1 1.436(6) . ?
C1 C6 1.398(6) . ?
C1 C2 1.416(6) . ?
C10 H10 0.9500 . ?
C10 C9 1.378(6) . ?
C9 C8 1.483(5) . ?
C9 C13 1.402(5) . ?
C4 H4 0.9500 . ?
C4 C3 1.399(6) . ?
C4 C5 1.395(6) . ?
C6 H6 0.9500 . ?
C6 C5 1.390(6) . ?
C3 H3A 0.9500 . ?
C3 C2 1.382(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C13 H13 0.9500 . ?
C13 C12 1.378(6) . ?
N4 C15 1.147(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.380(6) . ?
C12 H12 0.9500 . ?
C15 C16 1.428(9) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 Mo2 O11 78.36(8) . . ?
O8 Mo2 O10 152.89(11) . . ?
O8 Mo2 O9 86.71(12) . . ?
O10 Mo2 O11 75.31(8) . . ?
O9 Mo2 O11 75.12(8) . . ?
O9 Mo2 O10 80.46(12) . . ?
O7 Mo2 O11 78.13(9) . . ?
O7 Mo2 O8 94.16(13) . . ?
O7 Mo2 O10 86.70(13) . . ?
O7 Mo2 O9 152.49(12) . . ?
O6 Mo2 O11 175.24(10) . . ?
O6 Mo2 O8 105.02(14) . . ?
O6 Mo2 O10 100.91(13) . . ?
O6 Mo2 O9 101.55(13) . . ?
O6 Mo2 O7 104.73(13) . . ?
O15 Mo3 O11 75.64(8) 2_566 . ?
O15 Mo3 O7 81.89(12) 2_566 2_566 ?
O13 Mo3 O11 77.03(8) . . ?
O13 Mo3 O15 151.83(12) . 2_566 ?
O13 Mo3 O7 84.62(13) . 2_566 ?
O9 Mo3 O11 78.00(9) . . ?
O9 Mo3 O15 88.81(12) . 2_566 ?
O9 Mo3 O13 92.14(13) . . ?
O9 Mo3 O7 152.92(12) . 2_566 ?
O7 Mo3 O11 75.07(8) 2_566 . ?
O12 Mo3 O11 176.45(11) . . ?
O12 Mo3 O15 103.02(14) . 2_566 ?
O12 Mo3 O13 103.86(14) . . ?
O12 Mo3 O9 105.33(14) . . ?
O12 Mo3 O7 101.54(13) . 2_566 ?
O2 Mo1 N1 71.75(12) . . ?
O1 Mo1 O2 146.45(12) . . ?
O1 Mo1 N1 80.48(12) . . ?
O4 Mo1 O2 95.62(13) . . ?
O4 Mo1 O1 101.81(14) . . ?
O4 Mo1 N1 154.28(13) . . ?
O3 Mo1 O2 101.30(14) . . ?
O3 Mo1 O1 100.57(15) . . ?
O3 Mo1 O4 107.25(16) . . ?
O3 Mo1 N1 97.33(14) . . ?
O8 Mo4 O11 75.43(8) 2_566 . ?
O10 Mo4 O11 78.25(9) . . ?
O10 Mo4 O8 153.59(12) . 2_566 ?
O10 Mo4 O15 91.50(13) . . ?
O10 Mo4 O13 89.30(12) . . ?
O15 Mo4 O11 76.70(9) . . ?
O15 Mo4 O8 84.60(12) . 2_566 ?
O15 Mo4 O13 151.80(12) . . ?
O13 Mo4 O11 75.88(8) . . ?
O13 Mo4 O8 82.29(12) . 2_566 ?
O14 Mo4 O11 176.50(10) . . ?
O14 Mo4 O8 101.07(13) . 2_566 ?
O14 Mo4 O10 105.24(13) . . ?
O14 Mo4 O15 103.26(14) . . ?
O14 Mo4 O13 103.70(13) . . ?
C8 O2 Mo1 118.6(3) . . ?
Mo2 O11 Mo2 180.0 . 2_566 ?
Mo3 O11 Mo2 89.972(10) 2_566 2_566 ?
Mo3 O11 Mo2 90.027(10) 2_566 . ?
Mo3 O11 Mo2 89.973(10) . . ?
Mo3 O11 Mo2 90.028(10) . 2_566 ?
Mo3 O11 Mo3 180.0 . 2_566 ?
Mo4 O11 Mo2 90.157(11) 2_566 . ?
Mo4 O11 Mo2 89.843(11) . . ?
Mo4 O11 Mo2 89.843(11) 2_566 2_566 ?
Mo4 O11 Mo2 90.157(11) . 2_566 ?
Mo4 O11 Mo3 89.524(11) 2_566 2_566 ?
Mo4 O11 Mo3 89.526(11) . . ?
Mo4 O11 Mo3 90.475(11) . 2_566 ?
Mo4 O11 Mo3 90.475(11) 2_566 . ?
Mo4 O11 Mo4 180.0 2_566 . ?
Mo2 O8 Mo4 115.93(13) . 2_566 ?
Mo4 O10 Mo2 116.19(14) . . ?
Mo4 O15 Mo3 117.19(14) . 2_566 ?
Mo3 O13 Mo4 116.49(14) . . ?
Mo3 O9 Mo2 116.84(14) . . ?
Mo2 O7 Mo3 116.26(13) . 2_566 ?
C2 O1 Mo1 132.8(2) . . ?
C5 O5 C14 117.8(3) . . ?
C8 N2 N1 108.3(3) . . ?
C10 N3 H3 118.2 . . ?
C10 N3 C11 123.5(4) . . ?
C11 N3 H3 118.2 . . ?
N2 N1 Mo1 116.6(2) . . ?
C7 N1 Mo1 127.8(3) . . ?
C7 N1 N2 115.3(3) . . ?
N1 C7 H7 118.2 . . ?
N1 C7 C1 123.5(4) . . ?
C1 C7 H7 118.2 . . ?
C6 C1 C7 118.1(4) . . ?
C6 C1 C2 119.6(4) . . ?
C2 C1 C7 122.3(4) . . ?
N3 C10 H10 120.3 . . ?
N3 C10 C9 119.5(4) . . ?
C9 C10 H10 120.3 . . ?
C10 C9 C8 120.9(3) . . ?
C10 C9 C13 118.7(4) . . ?
C13 C9 C8 120.3(4) . . ?
O2 C8 C9 118.1(3) . . ?
N2 C8 O2 124.6(4) . . ?
N2 C8 C9 117.2(3) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C5 C4 C3 120.2(4) . . ?
C1 C6 H6 119.6 . . ?
C5 C6 C1 120.8(4) . . ?
C5 C6 H6 119.6 . . ?
C4 C3 H3A 119.6 . . ?
C2 C3 C4 120.9(4) . . ?
C2 C3 H3A 119.6 . . ?
O5 C14 H14A 109.5 . . ?
O5 C14 H14B 109.5 . . ?
O5 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C9 C13 H13 120.1 . . ?
C12 C13 C9 119.8(4) . . ?
C12 C13 H13 120.1 . . ?
O5 C5 C4 125.0(4) . . ?
O5 C5 C6 115.7(4) . . ?
C6 C5 C4 119.3(4) . . ?
O1 C2 C1 121.6(4) . . ?
O1 C2 C3 119.3(4) . . ?
C3 C2 C1 119.1(4) . . ?
N3 C11 H11 120.6 . . ?
N3 C11 C12 118.8(4) . . ?
C12 C11 H11 120.6 . . ?
C13 C12 C11 119.7(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
N4 C15 C16 178.1(6) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O2 C8 N2 -3.3(5) . . . . ?
Mo1 O2 C8 C9 178.2(2) . . . . ?
Mo1 O1 C2 C1 36.6(5) . . . . ?
Mo1 O1 C2 C3 -145.8(3) . . . . ?
Mo1 N1 C7 C1 -7.9(5) . . . . ?
O11 Mo2 O8 Mo4 3.04(11) . . . 2_566 ?
O11 Mo2 O7 Mo3 -6.30(12) . . . 2_566 ?
O11 Mo3 O13 Mo4 -9.15(12) . . . . ?
O11 Mo3 O9 Mo2 -2.19(12) . . . . ?
O11 Mo4 O10 Mo2 5.69(12) . . . . ?
O8 Mo2 O7 Mo3 70.87(17) . . . 2_566 ?
O8 Mo4 O10 Mo2 10.4(4) 2_566 . . . ?
O10 Mo2 O8 Mo4 17.0(4) . . . 2_566 ?
O10 Mo2 O7 Mo3 -81.97(16) . . . 2_566 ?
O15 Mo3 O13 Mo4 -23.5(3) 2_566 . . . ?
O15 Mo3 O9 Mo2 73.37(16) 2_566 . . . ?
O15 Mo4 O10 Mo2 -70.39(16) . . . . ?
O13 Mo3 O9 Mo2 -78.46(17) . . . . ?
O13 Mo4 O10 Mo2 81.41(16) . . . . ?
O9 Mo2 O8 Mo4 78.52(15) . . . 2_566 ?
O9 Mo2 O7 Mo3 -20.0(4) . . . 2_566 ?
O9 Mo3 O13 Mo4 68.02(17) . . . . ?
O7 Mo2 O8 Mo4 -73.93(16) . . . 2_566 ?
O7 Mo3 O13 Mo4 -85.03(16) 2_566 . . . ?
O7 Mo3 O9 Mo2 3.9(4) 2_566 . . . ?
O12 Mo3 O13 Mo4 174.38(15) . . . . ?
O12 Mo3 O9 Mo2 176.55(16) . . . . ?
O14 Mo4 O10 Mo2 -174.57(15) . . . . ?
N2 N1 C7 C1 178.5(3) . . . . ?
O6 Mo2 O8 Mo4 179.60(15) . . . 2_566 ?
O6 Mo2 O7 Mo3 177.60(16) . . . 2_566 ?
N3 C10 C9 C8 -179.9(3) . . . . ?
N3 C10 C9 C13 -0.7(5) . . . . ?
N3 C11 C12 C13 -0.2(6) . . . . ?
N1 N2 C8 O2 1.8(5) . . . . ?
N1 N2 C8 C9 -179.6(3) . . . . ?
N1 C7 C1 C6 173.9(4) . . . . ?
N1 C7 C1 C2 -8.8(6) . . . . ?
C7 C1 C6 C5 -179.2(4) . . . . ?
C7 C1 C2 O1 -2.3(6) . . . . ?
C7 C1 C2 C3 -179.9(4) . . . . ?
C1 C6 C5 O5 179.6(4) . . . . ?
C1 C6 C5 C4 -1.4(6) . . . . ?
C10 N3 C11 C12 -0.4(6) . . . . ?
C10 C9 C8 O2 1.7(5) . . . . ?
C10 C9 C8 N2 -177.0(3) . . . . ?
C10 C9 C13 C12 0.0(5) . . . . ?
C9 C13 C12 C11 0.4(6) . . . . ?
C8 N2 N1 Mo1 0.3(4) . . . . ?
C8 N2 N1 C7 174.7(3) . . . . ?
C8 C9 C13 C12 179.3(3) . . . . ?
C4 C3 C2 O1 -177.7(4) . . . . ?
C4 C3 C2 C1 -0.1(6) . . . . ?
C6 C1 C2 O1 175.0(4) . . . . ?
C6 C1 C2 C3 -2.6(6) . . . . ?
C3 C4 C5 O5 177.6(4) . . . . ?
C3 C4 C5 C6 -1.3(6) . . . . ?
C14 O5 C5 C4 5.3(6) . . . . ?
C14 O5 C5 C6 -175.8(4) . . . . ?
C13 C9 C8 O2 -177.6(3) . . . . ?
C13 C9 C8 N2 3.7(5) . . . . ?
C5 C4 C3 C2 2.0(6) . . . . ?
C2 C1 C6 C5 3.4(6) . . . . ?
C11 N3 C10 C9 0.9(6) . . . . ?

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.876
_oxdiff_exptl_absorpt_empirical_full_min 0.519
# start Validation Reply Form
_vrf_PLAT430_exp_2378            
;
PROBLEM: Short Inter D...A Contact  O2       ..O6       .       2.81 Ang.  
RESPONSE: cis-MoO2 moiety is slightly skewed leading to closer than 
expected distances between neighboring oxygen atoms. 
However, no indications of errors in modelling the cis-MoO2 
moiety were observed.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1Ha-2CH3COCH3
_database_code_depnum_ccdc_archive 'CCDC 2335833'
loop_
_audit_author_name
_audit_author_address
'Mirta Rubcic'
;University of Zagreb
Croatia
;
_audit_update_record             
;
2024-02-27 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-04-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
"[N'-(2-oxo-3-methoxybenzylidene)nicotinoylhydrazonium](acetone)dioxomolybdenum(vi) hexamolybdate acetone solvate"
_chemical_formula_moiety         'Mo6 O19, 2(C17 H18 Mo N3 O6), 2(C3 H6 O)'
_chemical_formula_sum            'C40 H48 Mo8 N6 O33'
_chemical_formula_weight         1908.36
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Mo4 O17 C18 N3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9721(3)
_cell_length_b                   10.7368(2)
_cell_length_c                   16.4964(4)
_cell_angle_alpha                104.858(2)
_cell_angle_beta                 104.620(2)
_cell_angle_gamma                94.020(2)
_cell_volume                     1470.73(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    14257
_cell_measurement_temperature    169.99
_cell_measurement_theta_max      80.0670
_cell_measurement_theta_min      2.8910
_shelx_estimated_absorpt_T_max   0.972
_shelx_estimated_absorpt_T_min   0.157
_exptl_absorpt_coefficient_mu    14.380
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.194
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.155
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             930
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 0 7 0.0361
5 0 -7 0.0494
1 4 5 0.0836
-1 -4 -6 0.1027
0 -6 6 0.0010
0 6 -6 0.0010

_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.002
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.3380 -0.3472 6.6207 -0.8530 0.5201 0.0434
5.3574 0.4048 -6.5477 0.8534 -0.5204 -0.0293
1.1271 4.0580 5.4518 -0.0106 0.0001 0.9999
-0.9263 -4.0344 -5.6828 0.0422 -0.0194 -0.9989
0.3745 -6.4506 6.3043 -0.6659 -0.7024 -0.2514
-0.3745 6.4506 -6.3043 0.6659 0.7024 0.2514

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18183
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.522
_diffrn_reflns_theta_min         2.887
_diffrn_ambient_temperature      169.99
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     69.00  97.00   0.50    0.05    --   48.02  52.00  97.00   56
  2  ω    138.00 165.00   0.50    0.19    --  113.25  61.00  30.00   54
  3  ω    102.00 151.00   0.50    0.19    --  113.25  45.00   0.00   98
  4  ω    103.00 133.00   0.50    0.19    --  113.25  61.00  30.00   60
  5  ω     99.00 175.00   0.50    0.19    --  113.25  61.00  60.00  152
  6  ω    114.00 178.00   0.50    0.19    --  113.25  52.00  97.00  128
  7  ω    126.00 175.00   0.50    0.19    --  113.25  45.00 120.00   98
  8  ω    142.00 172.00   0.50    0.19    --  113.25  30.00 150.00   60
  9  ω    101.00 149.00   0.50    0.19    --  113.25  45.00  90.00   96
 10  ω    114.00 158.00   0.50    0.19    --  113.25  30.00   0.00   88
 11  ω    113.00 144.00   0.50    0.19    --  113.25  30.00 -90.00   62
 12  ω    138.00 172.00   0.50    0.19    --  113.25  45.00-150.00   68
 13  ω    144.00 173.00   0.50    0.19    --  113.25  15.00-150.00   58
 14  ω    115.00 141.00   0.50    0.19    --  113.25  15.00-150.00   52
 15  ω    -20.00  25.00   0.50    0.05    --   48.02 -19.00-150.00   90
 16  ω    -21.00  59.00   0.50    0.05    --   48.02 -52.00 -47.00  160
 17  ω    -12.00  63.00   0.50    0.05    --   48.02 -57.00  90.00  150
 18  ω     42.00 109.00   0.50    0.19    --  113.25-125.00  60.00  134
 19  ω     93.00 118.00   0.50    0.19    --  113.25-134.00   1.06   50
 20  ω     46.00  72.00   0.50    0.19    --  113.25-134.00   1.06   52
 21  ω     85.00 111.00   0.50    0.19    --  113.25-125.00 -90.00   52
 22  ω     62.00 111.00   0.50    0.19    --  113.25-125.00-150.00   98
 23  ω     43.00  78.00   0.50    0.19    --  113.25-125.00-180.00   70
 24  ω     84.00 111.00   0.50    0.19    --  113.25-125.00-180.00   54
 25  ω     35.00  96.00   0.50    0.05    --   48.02-125.00 -30.00  122
 26  ω     69.00 110.00   0.50    0.19    --  113.25-125.00  90.00   82
 27  ω     84.00 110.00   0.50    0.19    --  113.25-125.00 150.00   52
 28  ω     45.00 104.00   0.50    0.19    --  113.25 -95.00  60.00  118
 29  ω     64.00 108.00   0.50    0.19    --  113.25-110.00  18.97   88
 30  ω     77.00 102.00   0.50    0.19    --  113.25 -95.00   0.00   50
 31  ω     42.00  69.00   0.50    0.19    --  113.25-108.00-100.20   54
 32  ω     45.00  79.00   0.50    0.19    --  113.25 -99.00-150.56   68
 33  ω     80.00 107.00   0.50    0.19    --  113.25-108.00-100.20   54
 34  ω     71.00 102.00   0.50    0.19    --  113.25 -95.00 -90.00   62
 35  ω     54.00 104.00   0.50    0.19    --  113.25 -95.00 -60.00  100
 36  ω     43.00  96.00   0.50    0.19    --  113.25 -95.00  90.00  106
 37  ω     46.00  71.00   0.50    0.19    --  113.25 -61.00  90.00   50
 38  ω     56.00  88.00   0.50    0.19    --  113.25 -77.00  90.00   64
 39  ω     73.00 101.00   0.50    0.19    --  113.25 -77.00 -60.00   56
 40  ω     44.00  69.00   0.50    0.19    --  113.25 -77.00 -60.00   50
 41  ω     43.00  69.00   0.50    0.19    --  113.25 -61.00 -60.00   52
 42  ω     44.00  70.00   0.50    0.19    --  113.25 -77.00-120.00   52
 43  ω     45.00  70.00   0.50    0.19    --  113.25 -61.00-120.00   50
 44  ω     42.00  68.00   0.50    0.19    --  113.25 -61.00 -90.00   52
 45  ω     42.00  68.00   0.50    0.19    --  113.25 -61.00 150.00   52
 46  ω    114.00 167.00   0.50    0.19    --  113.25 125.00 -90.00  106
 47  ω     96.00 140.00   0.50    0.19    --  113.25 125.00 -30.00   88
 48  ω    150.00 176.00   0.50    0.19    --  113.25 125.00 -30.00   52
 49  ω    -20.00  23.00   0.50    0.05    --  -48.02  52.00  97.00   86
 50  ω    -53.00 -23.00   0.50    0.05    --  -48.02  52.00  97.00   60
 51  ω    -56.00 -31.00   0.50    0.19    --  -91.75  52.00  97.00   50
 52  ω    -70.00 -22.00   0.50    0.19    --  -91.75  61.00 -90.00   96
 53  ω    -46.00 -21.00   0.50    0.19    --  -91.75  45.00-120.00   50
 54  ω    -51.00 -21.00   0.50    0.19    --  -91.75  45.00-150.00   60
 55  ω   -118.00 -65.00   0.50    0.05    --  -48.02 -52.00 -47.00  106
 56  ω   -120.00 -95.00   0.50    0.05    --  -48.02-125.00 -60.00   50
 57  ω   -119.00 -81.00   0.50    0.05    --  -48.02-125.00-120.00   76
 58  ω   -121.00 -96.00   0.50    0.19    --  -91.75 -52.00 -47.00   50
 59  ω   -111.00 -76.00   0.50    0.05    --  -48.02-125.00  90.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0846773000
_diffrn_orient_matrix_UB_12      0.0515922000
_diffrn_orient_matrix_UB_13      -0.0578610000
_diffrn_orient_matrix_UB_21      -0.1360409000
_diffrn_orient_matrix_UB_22      0.0743879000
_diffrn_orient_matrix_UB_23      -0.0272258000
_diffrn_orient_matrix_UB_31      0.0804999000
_diffrn_orient_matrix_UB_32      0.1196205000
_diffrn_orient_matrix_UB_33      0.0777350000
_diffrn_oxdiff_digest_frames     
;
017a254803ed035e4dbb6c008c31acfcde04474c95e
;
_diffrn_oxdiff_digest_hkl        
;
011e8965894199009e7d02648f50bc13e049c5
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5659
_reflns_number_total             6056
_reflns_odcompleteness_completeness 96.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.389
_refine_diff_density_min         -2.465
_refine_diff_density_rms         0.180
_refine_ls_extinction_coef       0.00063(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         6056
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0453
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0647P)²+5.8824P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1252
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Sof: C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C19(0.5) H19A(0.5)
 H19B(0.5) H19C(0.5)
 Fixed Uiso: H3(0.029) H7(0.028) H10(0.029) H6(0.032) H13(0.03) H11(0.033)
 H4(0.044) H5(0.04) H12(0.034) H16A(0.065) H16B(0.065) H16C(0.065) H17A(0.049)
 H17B(0.049) H17C(0.049) H20A(0.085) H20B(0.085) H20C(0.085) H14A(0.103)
 H14B(0.103) H14C(0.103) H21A(0.074) H21B(0.074) H21C(0.074) H19A(0.131)
 H19B(0.131) H19C(0.131)
 Fixed X: O11(0) H3(0.558754) H7(0.229358) H10(0.458911) H6(0.10687)
 H13(0.548532) H11(0.651168) H4(-0.008301) H5(-0.004699) H12(0.645205)
 H16A(0.306313) H16B(0.165058) H16C(0.18645) H17A(-0.119318) H17B(-0.075916)
 H17C(-0.123387) H20A(0.438) H20B(0.479433) H20C(0.615203) H14A(-0.068009)
 H14B(0.099195) H14C(0.052487) H21A(0.293833) H21B(0.236462) H21C(0.291663)
 H19A(0.614686) H19B(0.430426) H19C(0.525722)
 Fixed Y: O11(0.5) H3(0.859616) H7(1.037632) H10(0.907202) H6(1.175552)
 H13(0.55662) H11(0.676219) H4(1.067475) H5(1.216396) H12(0.516605)
 H16A(0.453075) H16B(0.358838) H16C(0.360837) H17A(0.411712) H17B(0.463517)
 H17C(0.561314) H20A(1.269152) H20B(1.266134) H20C(1.274673) H14A(0.872545)
 H14B(0.94226) H14C(0.788361) H21A(0.948473) H21B(1.072127) H21C(1.079801)
 H19A(1.098304) H19B(1.065962) H19C(0.956217)
 Fixed Z: O11(0) H3(0.182985) H7(0.480085) H10(0.296871) H6(0.574798)
 H13(0.3314) H11(0.13596) H4(0.770846) H5(0.689281) H12(0.208366)
 H16A(0.415659) H16B(0.340031) H16C(0.43967) H17A(0.370518) H17B(0.295446)
 H17C(0.372769) H20A(0.208933) H20B(0.119671) H20C(0.205973) H14A(0.799923)
 H14B(0.863792) H14C(0.842625) H21A(0.130374) H21B(0.10105) H21C(0.202561)
 H19A(0.05337) H19B(0.009922) H19C(0.03832)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo2 Mo 0.08980(4) 0.54764(4) 0.15044(2) 0.02275(13) Uani 1 1 d . . . . .
Mo1 Mo 0.38980(4) 0.73595(4) 0.56472(2) 0.02181(13) Uani 1 1 d . . . . .
Mo3 Mo 0.23090(5) 0.60779(5) -0.00219(3) 0.03574(15) Uani 1 1 d . . . . .
Mo4 Mo 0.10565(6) 0.30759(5) -0.01413(3) 0.03827(15) Uani 1 1 d . . . . .
O11 O 0.000000 0.500000 0.000000 0.0181(9) Uani 1 2 d S T P . .
O2 O 0.4545(4) 0.6899(3) 0.4536(2) 0.0239(7) Uani 1 1 d . . . . .
O1 O 0.2376(5) 0.8018(4) 0.6216(2) 0.0315(8) Uani 1 1 d . . . . .
O4 O 0.4031(4) 0.5912(4) 0.5876(2) 0.0289(8) Uani 1 1 d . . . . .
O9 O 0.1587(5) 0.3845(4) 0.1113(2) 0.0340(9) Uani 1 1 d . . . . .
O6 O 0.1479(4) 0.6286(3) 0.4603(2) 0.0254(7) Uani 1 1 d . . . . .
O12 O 0.1161(5) 0.5498(5) -0.1233(3) 0.0409(10) Uani 1 1 d . . . . .
O8 O 0.1538(5) 0.5850(4) 0.2601(2) 0.0339(9) Uani 1 1 d . . . . .
O10 O 0.2549(5) 0.6295(4) 0.1211(2) 0.0368(9) Uani 1 1 d . . . . .
O15 O 0.0203(6) 0.3087(5) -0.1329(3) 0.0459(11) Uani 1 1 d . . . . .
N3 N 0.5561(5) 0.8010(4) 0.2116(3) 0.0242(8) Uani 1 1 d . . . . .
H3 H 0.558754 0.859616 0.182985 0.029 Uiso 1 1 calc R . . . .
O14 O 0.2753(5) 0.4368(6) -0.0109(3) 0.0475(12) Uani 1 1 d . . . . .
O5 O 0.1044(7) 0.8426(4) 0.7462(3) 0.0470(12) Uani 1 1 d . . . . .
N2 N 0.3596(5) 0.8692(4) 0.4161(3) 0.0218(8) Uani 1 1 d . . . . .
N1 N 0.3130(5) 0.8798(4) 0.4914(2) 0.0208(8) Uani 1 1 d . . . . .
O3 O 0.5531(5) 0.8372(4) 0.6310(3) 0.0397(10) Uani 1 1 d . . . . .
O17 O -0.0969(6) 0.2561(4) -0.0099(3) 0.0462(11) Uani 1 1 d . . . . .
C1 C 0.1761(6) 0.9999(5) 0.5872(3) 0.0237(9) Uani 1 1 d . . . . .
C7 C 0.2406(6) 0.9775(5) 0.5138(3) 0.0231(9) Uani 1 1 d . . . . .
H7 H 0.229358 1.037632 0.480085 0.028 Uiso 1 1 calc R . . . .
C10 C 0.4974(6) 0.8271(5) 0.2801(3) 0.0239(9) Uani 1 1 d . . . . .
H10 H 0.458911 0.907202 0.296871 0.029 Uiso 1 1 calc R . . . .
C9 C 0.4932(5) 0.7368(5) 0.3264(3) 0.0207(9) Uani 1 1 d . . . . .
C8 C 0.4321(5) 0.7674(5) 0.4035(3) 0.0194(8) Uani 1 1 d . . . . .
C6 C 0.1068(6) 1.1151(5) 0.6080(3) 0.0265(10) Uani 1 1 d . . . . .
H6 H 0.106870 1.175552 0.574798 0.032 Uiso 1 1 calc R . . . .
C13 C 0.5497(6) 0.6197(5) 0.3003(3) 0.0248(10) Uani 1 1 d . . . . .
H13 H 0.548532 0.556620 0.331400 0.030 Uiso 1 1 calc R . . . .
C2 C 0.1756(6) 0.9121(5) 0.6367(3) 0.0252(10) Uani 1 1 d . . . . .
O13 O 0.3977(6) 0.6926(8) -0.0003(3) 0.072(2) Uani 1 1 d . . . . .
C11 C 0.6104(6) 0.6905(5) 0.1849(3) 0.0277(10) Uani 1 1 d . . . . .
H11 H 0.651168 0.676219 0.135960 0.033 Uiso 1 1 calc R . . . .
C4 C 0.0383(7) 1.0502(6) 0.7242(4) 0.0365(13) Uani 1 1 d . . . . .
H4 H -0.008301 1.067475 0.770846 0.044 Uiso 1 1 calc R . . . .
C5 C 0.0403(6) 1.1390(5) 0.6754(4) 0.0335(12) Uani 1 1 d . . . . .
H5 H -0.004699 1.216396 0.689281 0.040 Uiso 1 1 calc R . . . .
C12 C 0.6078(6) 0.5964(5) 0.2278(3) 0.0285(10) Uani 1 1 d . . . . .
H12 H 0.645205 0.516605 0.208366 0.034 Uiso 1 1 calc R . . . .
C3 C 0.1036(7) 0.9373(6) 0.7048(4) 0.0330(11) Uani 1 1 d . . . . .
C15 C 0.0978(6) 0.5184(5) 0.4107(3) 0.0242(9) Uani 1 1 d . . . . .
O16 O 0.1903(9) 0.1718(6) -0.0252(4) 0.083(2) Uani 1 1 d . . . . .
O7 O 0.5489(12) 1.0254(6) 0.1733(4) 0.107(3) Uani 1 1 d . . . . .
C16 C 0.1974(8) 0.4139(6) 0.4007(5) 0.0432(15) Uani 1 1 d . . . . .
H16A H 0.306313 0.453075 0.415659 0.065 Uiso 1 1 calc GR . . . .
H16B H 0.165058 0.358838 0.340031 0.065 Uiso 1 1 calc GR . . . .
H16C H 0.186450 0.360837 0.439670 0.065 Uiso 1 1 calc GR . . . .
C17 C -0.0697(6) 0.4859(6) 0.3578(4) 0.0327(11) Uani 1 1 d . . . . .
H17A H -0.119318 0.411712 0.370518 0.049 Uiso 1 1 calc GR . . . .
H17B H -0.075916 0.463517 0.295446 0.049 Uiso 1 1 calc GR . . . .
H17C H -0.123387 0.561314 0.372769 0.049 Uiso 1 1 calc GR . . . .
C20 C 0.5071(12) 1.2382(7) 0.1730(5) 0.057(2) Uani 1 1 d . . . . .
H20A H 0.438000 1.269152 0.208933 0.085 Uiso 1 1 calc GR . . . .
H20B H 0.479433 1.266134 0.119671 0.085 Uiso 1 1 calc GR . . . .
H20C H 0.615203 1.274673 0.205973 0.085 Uiso 1 1 calc GR . . . .
C18 C 0.4905(10) 1.0961(7) 0.1497(5) 0.065(3) Uani 1 1 d D . . . .
C14 C 0.0422(14) 0.8630(8) 0.8187(5) 0.068(3) Uani 1 1 d . . . . .
H14A H -0.068009 0.872545 0.799923 0.103 Uiso 1 1 calc GR . . . .
H14B H 0.099195 0.942260 0.863792 0.103 Uiso 1 1 calc GR . . . .
H14C H 0.052487 0.788361 0.842625 0.103 Uiso 1 1 calc GR . . . .
C21 C 0.3096(16) 1.0438(17) 0.1455(9) 0.050(3) Uani 0.5 1 d . . . A .
H21A H 0.293833 0.948473 0.130374 0.074 Uiso 0.5 1 calc GR . . . .
H21B H 0.236462 1.072127 0.101050 0.074 Uiso 0.5 1 calc GR . . . .
H21C H 0.291663 1.079801 0.202561 0.074 Uiso 0.5 1 calc GR . . . .
C19 C 0.518(3) 1.050(2) 0.0532(12) 0.087(8) Uani 0.5 1 d D . . A -1
H19A H 0.614686 1.098304 0.053370 0.131 Uiso 0.5 1 calc GR . . A -1
H19B H 0.430426 1.065962 0.009922 0.131 Uiso 0.5 1 calc GR . . A -1
H19C H 0.525722 0.956217 0.038320 0.131 Uiso 0.5 1 calc GR . . A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo2 O11 2.3134(4) . ?
Mo2 O9 1.908(4) . ?
Mo2 O12 1.944(4) 2_565 ?
Mo2 O8 1.683(4) . ?
Mo2 O10 1.897(4) . ?
Mo2 O15 1.933(4) 2_565 ?
Mo1 O2 2.014(3) . ?
Mo1 O1 1.920(4) . ?
Mo1 O4 1.696(4) . ?
Mo1 O6 2.398(4) . ?
Mo1 N1 2.238(4) . ?
Mo1 O3 1.697(4) . ?
Mo3 O11 2.3142(4) . ?
Mo3 O12 1.916(4) . ?
Mo3 O10 1.940(4) . ?
Mo3 O14 1.883(5) . ?
Mo3 O17 1.959(5) 2_565 ?
Mo3 O13 1.686(5) . ?
Mo4 O11 2.3152(4) . ?
Mo4 O9 1.939(4) . ?
Mo4 O15 1.920(4) . ?
Mo4 O14 1.967(6) . ?
Mo4 O17 1.886(5) . ?
Mo4 O16 1.681(5) . ?
O2 C8 1.307(6) . ?
O1 C2 1.336(6) . ?
O6 C15 1.231(6) . ?
N3 H3 0.8800 . ?
N3 C10 1.339(6) . ?
N3 C11 1.327(7) . ?
O5 C3 1.362(8) . ?
O5 C14 1.418(8) . ?
N2 N1 1.389(5) . ?
N2 C8 1.309(6) . ?
N1 C7 1.294(6) . ?
C1 C7 1.443(7) . ?
C1 C6 1.425(7) . ?
C1 C2 1.397(7) . ?
C7 H7 0.9500 . ?
C10 H10 0.9500 . ?
C10 C9 1.384(7) . ?
C9 C8 1.478(7) . ?
C9 C13 1.395(7) . ?
C6 H6 0.9500 . ?
C6 C5 1.368(8) . ?
C13 H13 0.9500 . ?
C13 C12 1.393(7) . ?
C2 C3 1.410(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.377(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.398(9) . ?
C4 C3 1.381(8) . ?
C5 H5 0.9500 . ?
C12 H12 0.9500 . ?
C15 C16 1.484(7) . ?
C15 C17 1.501(7) . ?
O7 C18 1.053(10) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20 C18 1.461(10) . ?
C18 C21 1.658(17) . ?
C18 C19 1.629(14) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O9 Mo2 O11 77.16(11) . . ?
O9 Mo2 O12 87.0(2) . 2_565 ?
O9 Mo2 O15 153.62(17) . 2_565 ?
O12 Mo2 O11 76.67(11) 2_565 . ?
O8 Mo2 O11 178.90(16) . . ?
O8 Mo2 O9 103.95(19) . . ?
O8 Mo2 O12 103.37(18) . 2_565 ?
O8 Mo2 O10 102.91(18) . . ?
O8 Mo2 O15 102.4(2) . 2_565 ?
O10 Mo2 O11 77.00(11) . . ?
O10 Mo2 O9 88.8(2) . . ?
O10 Mo2 O12 153.63(16) . 2_565 ?
O10 Mo2 O15 87.3(2) . 2_565 ?
O15 Mo2 O11 76.53(12) 2_565 . ?
O15 Mo2 O12 85.1(2) 2_565 2_565 ?
O2 Mo1 O6 78.92(13) . . ?
O2 Mo1 N1 71.93(14) . . ?
O1 Mo1 O2 147.39(15) . . ?
O1 Mo1 O6 76.96(15) . . ?
O1 Mo1 N1 80.98(15) . . ?
O4 Mo1 O2 97.92(16) . . ?
O4 Mo1 O1 101.58(17) . . ?
O4 Mo1 O6 85.22(16) . . ?
O4 Mo1 N1 159.55(17) . . ?
O4 Mo1 O3 106.0(2) . . ?
N1 Mo1 O6 75.53(13) . . ?
O3 Mo1 O2 98.68(19) . . ?
O3 Mo1 O1 100.7(2) . . ?
O3 Mo1 O6 168.75(17) . . ?
O3 Mo1 N1 93.25(18) . . ?
O12 Mo3 O11 77.17(12) . . ?
O12 Mo3 O10 153.30(16) . . ?
O12 Mo3 O17 86.8(2) . 2_565 ?
O10 Mo3 O11 76.19(11) . . ?
O10 Mo3 O17 85.2(2) . 2_565 ?
O14 Mo3 O11 77.33(14) . . ?
O14 Mo3 O12 88.3(2) . . ?
O14 Mo3 O10 87.5(2) . . ?
O14 Mo3 O17 153.5(2) . 2_565 ?
O17 Mo3 O11 76.20(13) 2_565 . ?
O13 Mo3 O11 177.2(3) . . ?
O13 Mo3 O12 104.4(2) . . ?
O13 Mo3 O10 102.1(2) . . ?
O13 Mo3 O14 104.9(3) . . ?
O13 Mo3 O17 101.6(3) . 2_565 ?
O9 Mo4 O11 76.54(11) . . ?
O9 Mo4 O14 85.53(18) . . ?
O15 Mo4 O11 76.73(13) . . ?
O15 Mo4 O9 153.17(17) . . ?
O15 Mo4 O14 85.7(2) . . ?
O14 Mo4 O11 75.76(13) . . ?
O17 Mo4 O11 77.53(14) . . ?
O17 Mo4 O9 87.39(19) . . ?
O17 Mo4 O15 89.1(2) . . ?
O17 Mo4 O14 153.3(2) . . ?
O16 Mo4 O11 177.1(3) . . ?
O16 Mo4 O9 103.8(2) . . ?
O16 Mo4 O15 102.7(2) . . ?
O16 Mo4 O14 101.3(3) . . ?
O16 Mo4 O17 105.4(4) . . ?
Mo2 O11 Mo2 180.0 . 2_565 ?
Mo2 O11 Mo3 89.898(14) 2_565 2_565 ?
Mo2 O11 Mo3 90.102(14) 2_565 . ?
Mo2 O11 Mo3 89.897(14) . . ?
Mo2 O11 Mo3 90.103(14) . 2_565 ?
Mo2 O11 Mo4 89.892(15) 2_565 2_565 ?
Mo2 O11 Mo4 89.893(15) . . ?
Mo2 O11 Mo4 90.108(15) . 2_565 ?
Mo2 O11 Mo4 90.108(15) 2_565 . ?
Mo3 O11 Mo3 180.0 2_565 . ?
Mo3 O11 Mo4 89.84(2) 2_565 . ?
Mo3 O11 Mo4 89.84(2) . 2_565 ?
Mo3 O11 Mo4 90.16(2) . . ?
Mo3 O11 Mo4 90.16(2) 2_565 2_565 ?
Mo4 O11 Mo4 180.0 . 2_565 ?
C8 O2 Mo1 118.6(3) . . ?
C2 O1 Mo1 136.4(3) . . ?
Mo2 O9 Mo4 116.41(19) . . ?
C15 O6 Mo1 136.0(3) . . ?
Mo3 O12 Mo2 116.06(19) . 2_565 ?
Mo2 O10 Mo3 116.84(19) . . ?
Mo4 O15 Mo2 116.5(2) . 2_565 ?
C10 N3 H3 118.6 . . ?
C11 N3 H3 118.6 . . ?
C11 N3 C10 122.8(4) . . ?
Mo3 O14 Mo4 116.7(2) . . ?
C3 O5 C14 118.4(6) . . ?
C8 N2 N1 108.1(4) . . ?
N2 N1 Mo1 115.9(3) . . ?
C7 N1 Mo1 128.1(3) . . ?
C7 N1 N2 115.8(4) . . ?
Mo4 O17 Mo3 116.4(2) . 2_565 ?
C6 C1 C7 118.1(5) . . ?
C2 C1 C7 122.6(4) . . ?
C2 C1 C6 119.3(5) . . ?
N1 C7 C1 123.6(5) . . ?
N1 C7 H7 118.2 . . ?
C1 C7 H7 118.2 . . ?
N3 C10 H10 120.2 . . ?
N3 C10 C9 119.6(5) . . ?
C9 C10 H10 120.2 . . ?
C10 C9 C8 119.4(4) . . ?
C10 C9 C13 119.1(4) . . ?
C13 C9 C8 121.4(4) . . ?
O2 C8 N2 125.1(4) . . ?
O2 C8 C9 117.1(4) . . ?
N2 C8 C9 117.8(4) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 C1 120.3(5) . . ?
C5 C6 H6 119.9 . . ?
C9 C13 H13 120.4 . . ?
C12 C13 C9 119.2(5) . . ?
C12 C13 H13 120.4 . . ?
O1 C2 C1 123.2(4) . . ?
O1 C2 C3 117.3(5) . . ?
C1 C2 C3 119.5(5) . . ?
N3 C11 H11 119.9 . . ?
N3 C11 C12 120.3(5) . . ?
C12 C11 H11 119.9 . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C3 C4 C5 120.4(5) . . ?
C6 C5 C4 120.4(5) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C13 C12 H12 120.4 . . ?
C11 C12 C13 119.1(5) . . ?
C11 C12 H12 120.4 . . ?
O5 C3 C2 114.5(5) . . ?
O5 C3 C4 125.4(5) . . ?
C4 C3 C2 120.2(6) . . ?
O6 C15 C16 122.5(5) . . ?
O6 C15 C17 119.8(5) . . ?
C16 C15 C17 117.7(5) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
O7 C18 C20 136.9(8) . . ?
O7 C18 C21 100.1(11) . . ?
O7 C18 C19 95.1(11) . . ?
C20 C18 C21 106.9(9) . . ?
C20 C18 C19 105.9(10) . . ?
C19 C18 C21 110.4(12) . . ?
O5 C14 H14A 109.5 . . ?
O5 C14 H14B 109.5 . . ?
O5 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O2 C8 N2 -5.4(6) . . . . ?
Mo1 O2 C8 C9 174.9(3) . . . . ?
Mo1 O1 C2 C1 21.6(8) . . . . ?
Mo1 O1 C2 C3 -160.0(4) . . . . ?
Mo1 O6 C15 C16 -4.1(8) . . . . ?
Mo1 O6 C15 C17 175.9(3) . . . . ?
Mo1 N1 C7 C1 -9.2(7) . . . . ?
O11 Mo2 O10 Mo3 -2.3(2) . . . . ?
O11 Mo3 O14 Mo4 1.34(18) . . . . ?
O11 Mo4 O17 Mo3 0.00(18) . . . 2_565 ?
O1 C2 C3 O5 -1.1(8) . . . . ?
O1 C2 C3 C4 179.5(5) . . . . ?
O9 Mo2 O10 Mo3 74.8(3) . . . . ?
O9 Mo4 O17 Mo3 76.8(2) . . . 2_565 ?
O12 Mo2 O10 Mo3 -5.9(6) 2_565 . . . ?
O12 Mo3 O14 Mo4 -75.9(2) . . . . ?
O8 Mo2 O10 Mo3 178.8(3) . . . . ?
O10 Mo3 O14 Mo4 77.7(2) . . . . ?
O15 Mo2 O10 Mo3 -79.1(3) 2_565 . . . ?
O15 Mo4 O17 Mo3 -76.6(3) . . . 2_565 ?
N3 C10 C9 C8 178.4(4) . . . . ?
N3 C10 C9 C13 -0.3(7) . . . . ?
N3 C11 C12 C13 -0.9(8) . . . . ?
O14 Mo4 O17 Mo3 2.1(6) . . . 2_565 ?
N2 N1 C7 C1 176.4(4) . . . . ?
N1 N2 C8 O2 0.5(6) . . . . ?
N1 N2 C8 C9 -179.8(4) . . . . ?
O17 Mo3 O14 Mo4 3.6(6) 2_565 . . . ?
C1 C6 C5 C4 -0.6(8) . . . . ?
C1 C2 C3 O5 177.4(5) . . . . ?
C1 C2 C3 C4 -2.0(8) . . . . ?
C7 C1 C6 C5 178.2(5) . . . . ?
C7 C1 C2 O1 1.5(8) . . . . ?
C7 C1 C2 C3 -176.9(5) . . . . ?
C10 N3 C11 C12 0.1(8) . . . . ?
C10 C9 C8 O2 -168.7(4) . . . . ?
C10 C9 C8 N2 11.6(6) . . . . ?
C10 C9 C13 C12 -0.4(7) . . . . ?
C9 C13 C12 C11 1.1(8) . . . . ?
C8 N2 N1 Mo1 4.1(5) . . . . ?
C8 N2 N1 C7 179.2(4) . . . . ?
C8 C9 C13 C12 -179.2(4) . . . . ?
C6 C1 C7 N1 176.5(5) . . . . ?
C6 C1 C2 O1 179.9(5) . . . . ?
C6 C1 C2 C3 1.5(7) . . . . ?
C13 C9 C8 O2 10.0(7) . . . . ?
C13 C9 C8 N2 -169.7(4) . . . . ?
C2 C1 C7 N1 -5.1(8) . . . . ?
C2 C1 C6 C5 -0.2(7) . . . . ?
O13 Mo3 O14 Mo4 179.6(2) . . . . ?
C11 N3 C10 C9 0.5(7) . . . . ?
C5 C4 C3 O5 -178.1(6) . . . . ?
C5 C4 C3 C2 1.2(9) . . . . ?
C3 C4 C5 C6 0.1(9) . . . . ?
O16 Mo4 O17 Mo3 -179.6(3) . . . 2_565 ?
C14 O5 C3 C2 176.6(7) . . . . ?
C14 O5 C3 C4 -4.1(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.603
_oxdiff_exptl_absorpt_empirical_full_min 0.639
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2Hw-2CH3COCH3
_database_code_depnum_ccdc_archive 'CCDC 2335830'
loop_
_audit_author_name
_audit_author_address
'Mirta Rubcic'
;University of Zagreb
Croatia
;
_audit_update_record             
;
2024-02-27 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-05-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'bis((aquo)-dioxo-(N-(2-oxy-3-methoxybenzylidene)nicotinylhydrazonato)-molybdenum(vi)) hexamolybdate acetone solvate'
_chemical_formula_moiety         'Mo6 O19, 2(C14 H14 Mo N3 O6), 2(C3 H6 O)'
_chemical_formula_sum            'C34 H40 Mo8 N6 O33'
_chemical_formula_weight         1828.24
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1475(4)
_cell_length_b                   10.3331(5)
_cell_length_c                   14.6331(5)
_cell_angle_alpha                108.527(4)
_cell_angle_beta                 92.219(3)
_cell_angle_gamma                110.565(4)
_cell_volume                     1342.45(11)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    2947
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.1540
_cell_measurement_theta_min      4.4020
_shelx_estimated_absorpt_T_max   0.945
_shelx_estimated_absorpt_T_min   0.832
_exptl_absorpt_coefficient_mu    1.907
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.261
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             886
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0874
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17550
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_min         3.977
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4379
_reflns_number_total             7018
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         7018
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0517
_refine_ls_restrained_S_all      0.962
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0361P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0898
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H7(0.044) H3(0.058) H3A(0.043) H13(0.053) H10(0.048) H5(0.049)
 H12(0.061) H14A(0.08) H14B(0.08) H14C(0.08) H11(0.066) H17A(0.096) H17B(0.096)
 H17C(0.096) H15A(0.154) H15B(0.154) H15C(0.154) H6A(0.051) H6B(0.051) H6(0.047)
 Fixed X: H7(0.434968) H3A(0.767833) H13(-0.004875) H10(-0.139395)
 H5(0.916918) H12(-0.241949) H14A(1.136023) H14B(0.996908) H14C(0.985292) H11(-
 0.422688) H17A(0.341548) H17B(0.347595) H17C(0.245302) H15A(0.523053)
 H15B(0.552492) H15C(0.651654) O11(1) H6(0.687405)
 Fixed Y: H7(0.160398) H3A(0.220495) H13(0.048573) H10(-0.059644) H5(0.330678)
 H12(-0.03911) H14A(0.355886) H14B(0.388645) H14C(0.221772) H11(-0.143816)
 H17A(0.443788) H17B(0.597827) H17C(0.52333) H15A(0.447752) H15B(0.53078)
 H15C(0.605228) O11(0.5) H6(0.260371)
 Fixed Z: H7(0.18402) H3A(0.49658) H13(0.102109) H10(0.332851) H5(0.268133)
 H12(0.028271) H14A(0.543041) H14B(0.570404) H14C(0.522537) H11(0.105587)
 H17A(0.33854) H17B(0.41373) H17C(0.309641) H15A(0.268916) H15B(0.191774)
 H15C(0.297065) O11(0) H6(0.192696)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O17 O 1.1179(4) 0.7417(3) 0.1586(2) 0.0396(8) Uani 1 1 d . . . . .
O5 O 1.0034(4) 0.3265(4) 0.4280(3) 0.0509(10) Uani 1 1 d . . . . .
O7 O 0.4730(4) 0.7410(4) 0.2997(3) 0.0505(10) Uani 1 1 d . . . . .
C9 C -0.0485(5) 0.0003(5) 0.2241(3) 0.0333(11) Uani 1 1 d . . . . .
C4 C 0.8638(6) 0.2835(5) 0.3904(4) 0.0386(12) Uani 1 1 d . . . . .
C7 C 0.4445(6) 0.1608(5) 0.2490(3) 0.0366(12) Uani 1 1 d . . . . .
H7 H 0.434968 0.160398 0.184020 0.044 Uiso 1 1 calc R . . . .
N3 N -0.2932(5) -0.1081(5) 0.2248(4) 0.0484(12) Uani 1 1 d D . . . .
H3 H -0.360(4) -0.164(5) 0.244(4) 0.058 Uiso 1 1 d DR . . . .
C3 C 0.7504(6) 0.2295(5) 0.4351(3) 0.0357(12) Uani 1 1 d . . . . .
H3A H 0.767833 0.220495 0.496580 0.043 Uiso 1 1 calc R . . . .
C13 C -0.0798(6) 0.0075(6) 0.1340(4) 0.0442(14) Uani 1 1 d . . . . .
H13 H -0.004875 0.048573 0.102109 0.053 Uiso 1 1 calc R . . . .
C10 C -0.1589(6) -0.0568(5) 0.2696(4) 0.0400(13) Uani 1 1 d . . . . .
H10 H -0.139395 -0.059644 0.332851 0.048 Uiso 1 1 calc R . . . .
C5 C 0.8389(6) 0.2946(5) 0.2993(4) 0.0407(13) Uani 1 1 d . . . . .
H5 H 0.916918 0.330678 0.268133 0.049 Uiso 1 1 calc R . . . .
C12 C -0.2196(7) -0.0447(6) 0.0902(4) 0.0510(15) Uani 1 1 d . . . . .
H12 H -0.241949 -0.039110 0.028271 0.061 Uiso 1 1 calc R . . . .
C14 C 1.0327(6) 0.3229(6) 0.5235(4) 0.0532(15) Uani 1 1 d . . . . .
H14A H 1.136023 0.355886 0.543041 0.080 Uiso 1 1 calc R . . . .
H14B H 0.996908 0.388645 0.570404 0.080 Uiso 1 1 calc R . . . .
H14C H 0.985292 0.221772 0.522537 0.080 Uiso 1 1 calc R . . . .
C11 C -0.3258(7) -0.1046(6) 0.1362(4) 0.0553(16) Uani 1 1 d . . . . .
H11 H -0.422688 -0.143816 0.105587 0.066 Uiso 1 1 calc R . . . .
C17 C 0.3373(7) 0.5394(6) 0.3445(4) 0.0640(18) Uani 1 1 d . . . . .
H17A H 0.341548 0.443788 0.338540 0.096 Uiso 1 1 calc R . . . .
H17B H 0.347595 0.597827 0.413730 0.096 Uiso 1 1 calc R . . . .
H17C H 0.245302 0.523330 0.309641 0.096 Uiso 1 1 calc R . . . .
C16 C 0.4551(6) 0.6202(7) 0.3014(4) 0.0523(15) Uani 1 1 d . . . . .
C15 C 0.5543(8) 0.5443(8) 0.2613(7) 0.102(3) Uani 1 1 d . . . . .
H15A H 0.523053 0.447752 0.268916 0.154 Uiso 1 1 calc R . . . .
H15B H 0.552492 0.530780 0.191774 0.154 Uiso 1 1 calc R . . . .
H15C H 0.651654 0.605228 0.297065 0.154 Uiso 1 1 calc R . . . .
Mo4 Mo 0.94045(5) 0.58198(5) 0.15265(3) 0.03688(12) Uani 1 1 d . . . . .
Mo1 Mo 0.31362(5) 0.12408(5) 0.43822(3) 0.03576(12) Uani 1 1 d . . . . .
Mo3 Mo 1.14172(5) 0.40153(5) 0.06048(3) 0.04069(13) Uani 1 1 d . . . . .
Mo2 Mo 0.80471(5) 0.27786(5) -0.03904(3) 0.03992(13) Uani 1 1 d . . . . .
N2 N 0.2024(5) 0.0892(4) 0.2272(3) 0.0378(10) Uani 1 1 d . . . . .
O14 O 1.0631(4) 0.4787(4) 0.1705(2) 0.0427(9) Uani 1 1 d . . . . .
O2 O 0.1154(4) 0.0461(3) 0.3628(2) 0.0379(8) Uani 1 1 d . . . . .
O10 O 0.7933(4) 0.3912(4) 0.0910(2) 0.0426(9) Uani 1 1 d . . . . .
O4 O 0.2627(4) 0.0654(4) 0.5324(2) 0.0486(10) Uani 1 1 d . . . . .
O11 O 1.000000 0.500000 0.000000 0.0291(10) Uani 1 2 d S T P . .
O1 O 0.5061(4) 0.1321(4) 0.4370(2) 0.0412(9) Uani 1 1 d . . . . .
O9 O 0.9484(4) 0.2365(4) 0.0127(2) 0.0441(9) Uani 1 1 d . . . . .
O12 O 0.8461(4) 0.6544(4) 0.0788(2) 0.0399(9) Uani 1 1 d . . . . .
O16 O 1.2732(4) 0.5916(4) 0.0785(2) 0.0419(9) Uani 1 1 d . . . . .
C8 C 0.0982(6) 0.0500(5) 0.2737(3) 0.0342(11) Uani 1 1 d . . . . .
N1 N 0.3310(5) 0.1249(4) 0.2860(3) 0.0348(10) Uani 1 1 d . . . . .
C2 C 0.6123(6) 0.1886(5) 0.3916(3) 0.0342(12) Uani 1 1 d . . . . .
O6 O 0.2723(4) -0.1270(4) 0.3512(3) 0.0422(9) Uani 1 1 d D . . . .
H6A H 0.345(4) -0.142(6) 0.346(4) 0.051 Uiso 1 1 d DR . . . .
H6B H 0.227(5) -0.163(5) 0.296(2) 0.051 Uiso 1 1 d DR . . . .
O13 O 0.9025(4) 0.6432(4) 0.2649(2) 0.0520(10) Uani 1 1 d . . . . .
C1 C 0.5848(6) 0.2015(5) 0.2990(3) 0.0342(11) Uani 1 1 d . . . . .
O8 O 0.6578(4) 0.1226(4) -0.0669(3) 0.0569(11) Uani 1 1 d . . . . .
O15 O 1.2387(4) 0.3220(4) 0.1004(3) 0.0581(11) Uani 1 1 d . . . . .
C6 C 0.7028(6) 0.2535(5) 0.2552(4) 0.0388(13) Uani 1 1 d . . . . .
H6 H 0.687405 0.260371 0.192696 0.047 Uiso 1 1 calc R . . . .
O3 O 0.3480(4) 0.3059(4) 0.4806(3) 0.0532(10) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O17 Mo4 1.945(3) . ?
O17 Mo2 1.927(3) 2_765 ?
O5 C4 1.360(6) . ?
O5 C14 1.433(6) . ?
O7 C16 1.206(6) . ?
C9 C13 1.376(6) . ?
C9 C10 1.375(7) . ?
C9 C8 1.466(7) . ?
C4 C3 1.379(7) . ?
C4 C5 1.395(7) . ?
C7 H7 0.9500 . ?
C7 N1 1.278(6) . ?
C7 C1 1.429(7) . ?
N3 H3 0.844(19) . ?
N3 C10 1.331(7) . ?
N3 C11 1.340(7) . ?
C3 H3A 0.9500 . ?
C3 C2 1.375(7) . ?
C13 H13 0.9500 . ?
C13 C12 1.374(8) . ?
C10 H10 0.9500 . ?
C5 H5 0.9500 . ?
C5 C6 1.360(7) . ?
C12 H12 0.9500 . ?
C12 C11 1.359(8) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C11 H11 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 C16 1.488(8) . ?
C16 C15 1.510(9) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
Mo4 O14 1.960(3) . ?
Mo4 O10 1.904(3) . ?
Mo4 O11 2.3095(4) . ?
Mo4 O12 1.893(3) . ?
Mo4 O13 1.675(3) . ?
Mo1 O2 2.009(3) . ?
Mo1 O4 1.702(3) . ?
Mo1 O1 1.926(4) . ?
Mo1 N1 2.243(4) . ?
Mo1 O6 2.371(4) . ?
Mo1 O3 1.679(4) . ?
Mo3 O14 1.896(3) . ?
Mo3 O11 2.3213(4) . ?
Mo3 O9 2.008(4) . ?
Mo3 O12 1.955(3) 2_765 ?
Mo3 O16 1.874(3) . ?
Mo3 O15 1.677(3) . ?
Mo2 O10 1.924(3) . ?
Mo2 O11 2.3250(5) . ?
Mo2 O9 1.854(4) . ?
Mo2 O16 1.996(3) 2_765 ?
Mo2 O8 1.679(4) . ?
N2 C8 1.295(6) . ?
N2 N1 1.398(5) . ?
O2 C8 1.324(5) . ?
O1 C2 1.343(6) . ?
C2 C1 1.429(6) . ?
O6 H6A 0.807(19) . ?
O6 H6B 0.815(19) . ?
C1 C6 1.401(7) . ?
C6 H6 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Mo2 O17 Mo4 115.99(15) 2_765 . ?
C4 O5 C14 116.6(4) . . ?
C13 C9 C8 122.7(5) . . ?
C10 C9 C13 118.9(5) . . ?
C10 C9 C8 118.3(4) . . ?
O5 C4 C3 124.7(5) . . ?
O5 C4 C5 115.3(5) . . ?
C3 C4 C5 120.0(5) . . ?
N1 C7 H7 117.9 . . ?
N1 C7 C1 124.2(4) . . ?
C1 C7 H7 117.9 . . ?
C10 N3 H3 120(4) . . ?
C10 N3 C11 122.2(5) . . ?
C11 N3 H3 116(4) . . ?
C4 C3 H3A 119.6 . . ?
C2 C3 C4 120.7(5) . . ?
C2 C3 H3A 119.6 . . ?
C9 C13 H13 120.1 . . ?
C12 C13 C9 119.9(6) . . ?
C12 C13 H13 120.1 . . ?
C9 C10 H10 120.1 . . ?
N3 C10 C9 119.7(5) . . ?
N3 C10 H10 120.1 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 119.9(5) . . ?
C6 C5 H5 120.0 . . ?
C13 C12 H12 120.3 . . ?
C11 C12 C13 119.5(5) . . ?
C11 C12 H12 120.3 . . ?
O5 C14 H14A 109.5 . . ?
O5 C14 H14B 109.5 . . ?
O5 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C11 C12 119.8(6) . . ?
N3 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
O7 C16 C17 122.3(6) . . ?
O7 C16 C15 121.1(6) . . ?
C17 C16 C15 116.5(6) . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O17 Mo4 O14 85.09(15) . . ?
O17 Mo4 O11 76.76(9) . . ?
O14 Mo4 O11 76.15(9) . . ?
O10 Mo4 O17 153.43(14) . . ?
O10 Mo4 O14 86.49(15) . . ?
O10 Mo4 O11 76.77(10) . . ?
O12 Mo4 O17 88.10(14) . . ?
O12 Mo4 O14 153.70(13) . . ?
O12 Mo4 O10 88.39(15) . . ?
O12 Mo4 O11 77.56(10) . . ?
O13 Mo4 O17 101.93(16) . . ?
O13 Mo4 O14 102.61(16) . . ?
O13 Mo4 O10 104.48(16) . . ?
O13 Mo4 O11 178.24(13) . . ?
O13 Mo4 O12 103.65(16) . . ?
O2 Mo1 N1 71.67(14) . . ?
O2 Mo1 O6 77.46(13) . . ?
O4 Mo1 O2 95.74(16) . . ?
O4 Mo1 O1 104.06(16) . . ?
O4 Mo1 N1 161.05(16) . . ?
O4 Mo1 O6 84.84(15) . . ?
O1 Mo1 O2 147.31(14) . . ?
O1 Mo1 N1 82.00(14) . . ?
O1 Mo1 O6 78.70(14) . . ?
N1 Mo1 O6 78.71(13) . . ?
O3 Mo1 O2 100.14(16) . . ?
O3 Mo1 O4 105.37(18) . . ?
O3 Mo1 O1 99.35(17) . . ?
O3 Mo1 N1 91.05(16) . . ?
O3 Mo1 O6 169.74(16) . . ?
O14 Mo3 O11 77.04(10) . . ?
O14 Mo3 O9 85.47(15) . . ?
O14 Mo3 O12 152.75(14) . 2_765 ?
O9 Mo3 O11 75.25(9) . . ?
O12 Mo3 O11 76.12(9) 2_765 . ?
O12 Mo3 O9 83.27(14) 2_765 . ?
O16 Mo3 O14 90.72(15) . . ?
O16 Mo3 O11 78.20(10) . . ?
O16 Mo3 O9 153.36(14) . . ?
O16 Mo3 O12 88.39(14) . 2_765 ?
O15 Mo3 O14 104.13(16) . . ?
O15 Mo3 O11 177.16(14) . . ?
O15 Mo3 O9 102.20(17) . . ?
O15 Mo3 O12 102.47(16) . 2_765 ?
O15 Mo3 O16 104.30(18) . . ?
O17 Mo2 O11 76.71(10) 2_765 . ?
O17 Mo2 O16 84.55(14) 2_765 2_765 ?
O10 Mo2 O17 152.24(14) . 2_765 ?
O10 Mo2 O11 76.02(10) . . ?
O10 Mo2 O16 83.90(14) . 2_765 ?
O9 Mo2 O17 89.75(15) . 2_765 ?
O9 Mo2 O10 89.57(15) . . ?
O9 Mo2 O11 77.97(11) . . ?
O9 Mo2 O16 153.81(14) . 2_765 ?
O16 Mo2 O11 75.84(10) 2_765 . ?
O8 Mo2 O17 104.38(16) . 2_765 ?
O8 Mo2 O10 102.60(16) . . ?
O8 Mo2 O11 176.85(14) . . ?
O8 Mo2 O9 104.93(17) . . ?
O8 Mo2 O16 101.25(17) . 2_765 ?
C8 N2 N1 109.0(4) . . ?
Mo3 O14 Mo4 116.52(15) . . ?
C8 O2 Mo1 119.4(3) . . ?
Mo4 O10 Mo2 117.39(17) . . ?
Mo4 O11 Mo4 180.0 2_765 . ?
Mo4 O11 Mo3 90.189(16) 2_765 2_765 ?
Mo4 O11 Mo3 89.810(16) . 2_765 ?
Mo4 O11 Mo3 90.189(16) . . ?
Mo4 O11 Mo3 89.812(16) 2_765 . ?
Mo4 O11 Mo2 89.782(17) 2_765 2_765 ?
Mo4 O11 Mo2 90.218(17) 2_765 . ?
Mo4 O11 Mo2 90.218(17) . 2_765 ?
Mo4 O11 Mo2 89.782(17) . . ?
Mo3 O11 Mo3 180.0 . 2_765 ?
Mo3 O11 Mo2 90.089(18) 2_765 2_765 ?
Mo3 O11 Mo2 90.088(18) . . ?
Mo3 O11 Mo2 89.911(18) 2_765 . ?
Mo3 O11 Mo2 89.911(18) . 2_765 ?
Mo2 O11 Mo2 180.0 2_765 . ?
C2 O1 Mo1 134.2(3) . . ?
Mo2 O9 Mo3 116.67(16) . . ?
Mo4 O12 Mo3 116.33(16) . 2_765 ?
Mo3 O16 Mo2 116.02(17) . 2_765 ?
N2 C8 C9 118.7(4) . . ?
N2 C8 O2 123.9(5) . . ?
O2 C8 C9 117.3(5) . . ?
C7 N1 Mo1 127.7(3) . . ?
C7 N1 N2 116.8(4) . . ?
N2 N1 Mo1 115.4(3) . . ?
C3 C2 C1 120.1(5) . . ?
O1 C2 C3 118.0(4) . . ?
O1 C2 C1 121.8(5) . . ?
Mo1 O6 H6A 113(4) . . ?
Mo1 O6 H6B 116(4) . . ?
H6A O6 H6B 106(6) . . ?
C7 C1 C2 123.5(5) . . ?
C6 C1 C7 119.3(4) . . ?
C6 C1 C2 117.3(5) . . ?
C5 C6 C1 122.0(5) . . ?
C5 C6 H6 119.0 . . ?
C1 C6 H6 119.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O17 Mo4 O12 Mo3 80.63(19) . . . 2_765 ?
O17 Mo2 O9 Mo3 77.68(19) 2_765 . . . ?
O5 C4 C3 C2 -180.0(4) . . . . ?
O5 C4 C5 C6 179.6(4) . . . . ?
C9 C13 C12 C11 -0.7(8) . . . . ?
C4 C3 C2 O1 177.8(4) . . . . ?
C4 C3 C2 C1 0.1(7) . . . . ?
C4 C5 C6 C1 0.8(8) . . . . ?
C7 C1 C6 C5 179.7(5) . . . . ?
C3 C4 C5 C6 0.7(7) . . . . ?
C3 C2 C1 C7 179.7(4) . . . . ?
C3 C2 C1 C6 1.4(7) . . . . ?
C13 C9 C10 N3 2.1(7) . . . . ?
C13 C9 C8 N2 -6.8(7) . . . . ?
C13 C9 C8 O2 176.0(4) . . . . ?
C13 C12 C11 N3 1.9(8) . . . . ?
C10 C9 C13 C12 -1.3(7) . . . . ?
C10 C9 C8 N2 172.8(4) . . . . ?
C10 C9 C8 O2 -4.5(6) . . . . ?
C10 N3 C11 C12 -1.2(8) . . . . ?
C5 C4 C3 C2 -1.2(7) . . . . ?
C14 O5 C4 C3 -4.0(7) . . . . ?
C14 O5 C4 C5 177.2(4) . . . . ?
C11 N3 C10 C9 -0.9(8) . . . . ?
Mo1 O2 C8 C9 -176.3(3) . . . . ?
Mo1 O2 C8 N2 6.6(6) . . . . ?
Mo1 O1 C2 C3 153.5(4) . . . . ?
Mo1 O1 C2 C1 -28.8(7) . . . . ?
O14 Mo4 O12 Mo3 5.7(4) . . . 2_765 ?
O14 Mo3 O16 Mo2 -74.93(18) . . . 2_765 ?
O10 Mo4 O12 Mo3 -73.04(19) . . . 2_765 ?
O10 Mo2 O9 Mo3 -74.57(19) . . . . ?
O11 Mo4 O12 Mo3 3.76(14) . . . 2_765 ?
O11 Mo3 O14 Mo4 -2.64(14) . . . . ?
O11 Mo3 O16 Mo2 1.67(13) . . . 2_765 ?
O11 Mo2 O9 Mo3 1.22(14) . . . . ?
O1 C2 C1 C7 2.1(7) . . . . ?
O1 C2 C1 C6 -176.2(4) . . . . ?
O9 Mo3 O14 Mo4 -78.53(19) . . . . ?
O9 Mo3 O16 Mo2 6.4(4) . . . 2_765 ?
O12 Mo3 O14 Mo4 -12.8(4) 2_765 . . . ?
O12 Mo3 O16 Mo2 77.83(18) 2_765 . . 2_765 ?
O16 Mo3 O14 Mo4 75.08(19) . . . . ?
O16 Mo2 O9 Mo3 0.6(4) 2_765 . . . ?
C8 C9 C13 C12 178.2(5) . . . . ?
C8 C9 C10 N3 -177.4(4) . . . . ?
C8 N2 N1 C7 177.5(4) . . . . ?
C8 N2 N1 Mo1 -5.8(5) . . . . ?
N1 C7 C1 C2 8.2(8) . . . . ?
N1 C7 C1 C6 -173.4(5) . . . . ?
N1 N2 C8 C9 -177.0(4) . . . . ?
N1 N2 C8 O2 0.1(6) . . . . ?
C2 C1 C6 C5 -1.9(7) . . . . ?
O13 Mo4 O12 Mo3 -177.6(2) . . . 2_765 ?
C1 C7 N1 Mo1 3.2(7) . . . . ?
C1 C7 N1 N2 179.5(4) . . . . ?
O8 Mo2 O9 Mo3 -177.49(18) . . . . ?
O15 Mo3 O14 Mo4 -180.0(2) . . . . ?
O15 Mo3 O16 Mo2 -179.72(18) . . . 2_765 ?

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         17 Note  
RESPONSE: Low-angle reflections are shadowed by beam-stop, and not included 
          in integration.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3Hw-2CH3COCH3
_database_code_depnum_ccdc_archive 'CCDC 2335834'
loop_
_audit_author_name
_audit_author_address
'Mirta Rubcic'
;University of Zagreb
Croatia
;
_audit_update_record             
;
2024-02-27 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-05-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Mo6 O19, 2(C14 H14 Mo N3 O6), 2(C3 H6 O)'
_chemical_formula_sum            'C34 H40 Mo8 N6 O33'
_chemical_formula_weight         1828.24
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Mo C H N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6083(8)
_cell_length_b                   10.7813(6)
_cell_length_c                   12.8485(6)
_cell_angle_alpha                106.660(5)
_cell_angle_beta                 106.352(6)
_cell_angle_gamma                99.224(5)
_cell_volume                     1303.61(15)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    8960
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      78.9620
_cell_measurement_theta_min      3.8490
_shelx_estimated_absorpt_T_max   0.498
_shelx_estimated_absorpt_T_min   0.247
_exptl_absorpt_coefficient_mu    16.182
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.329
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             886
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0926
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17776
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.310
_diffrn_reflns_theta_min         3.828
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    105.00 139.00   0.50    0.05    --  113.25  30.00  60.00   68
  2  ω    118.00 174.00   0.50    0.05    --  113.25  45.00 -30.00  112
  3  ω    120.00 178.00   0.50    0.05    --  113.25  45.00 -90.00  116
  4  ω    149.00 175.00   0.50    0.05    --  113.25  61.00-120.00   52
  5  ω     98.00 138.00   0.50    0.05    --  113.25  61.00-120.00   80
  6  ω    100.00 126.00   0.50    0.05    --  113.25  15.00-150.00   52
  7  ω    131.00 178.00   0.50    0.05    --  113.25  15.00-150.00   94
  8  ω    137.00 163.00   0.50    0.05    --  113.25  30.00-120.00   52
  9  ω    127.00 177.00   0.50    0.05    --  113.25   0.00  90.00  100
 10  ω     54.00 118.00   0.50    0.05    --  113.25   0.00  90.00  128
 11  ω     77.00 103.00   0.50    0.05    --  113.25 -95.00 -30.00   52
 12  ω     80.00 107.00   0.50    0.05    --  113.25-125.00   0.00   54
 13  ω     92.00 133.00   0.50    0.05    --  113.25-156.00  14.19   82
 14  ω     85.00 110.00   0.50    0.05    --  113.25-125.00 -90.00   50
 15  ω     56.00  84.00   0.50    0.05    --  113.25-156.00  14.19   56
 16  ω     63.00 111.00   0.50    0.05    --  113.25-125.00 -60.00   96
 17  ω     46.00  78.00   0.50    0.05    --  113.25-125.00 -90.00   64
 18  ω     46.00  74.00   0.50    0.05    --  113.25-125.00   0.00   56
 19  ω     48.00  77.00   0.50    0.05    --  113.25-125.00  60.00   58
 20  ω     81.00 106.00   0.50    0.05    --  113.25-125.00 120.00   50
 21  ω     52.00 110.00   0.50    0.05    --  113.25-125.00 150.00  116
 22  ω     47.00  75.00   0.50    0.05    --  113.25-125.00 120.00   56
 23  ω     86.00 111.00   0.50    0.05    --  113.25-125.00  60.00   50
 24  ω     84.00 109.00   0.50    0.05    --  113.25-115.00  79.31   50
 25  ω     42.00  74.00   0.50    0.05    --  113.25-115.00  79.31   64
 26  ω     83.00 108.00   0.50    0.05    --  113.25-106.00  39.46   50
 27  ω     82.00 111.00   0.50    0.05    --  113.25-125.00-180.00   58
 28  ω     84.00 109.00   0.50    0.05    --  113.25-113.00-176.00   50
 29  ω     51.00  77.00   0.50    0.05    --  113.25-113.00-176.00   52
 30  ω     26.00  67.00   0.50    0.05    --   48.02-113.00-176.00   82
 31  ω     43.00  97.00   0.50    0.05    --  113.25 -95.00   0.00  108
 32  ω     57.00 106.00   0.50    0.05    --  113.25 -95.00 150.00   98
 33  ω     42.00  77.00   0.50    0.05    --  113.25 -95.00 -60.00   70
 34  ω     66.00  92.00   0.50    0.05    --  113.25 -95.00-120.00   52
 35  ω     42.00  71.00   0.50    0.05    --  113.25 -61.00-180.00   58
 36  ω     80.00 105.00   0.50    0.05    --  113.25 -77.00-180.00   50
 37  ω     80.00 105.00   0.50    0.05    --  113.25 -77.00  30.00   50
 38  ω     72.00 104.00   0.50    0.05    --  113.25 -77.00 150.00   64
 39  ω     46.00  71.00   0.50    0.05    --  113.25 -61.00 150.00   50
 40  ω     44.00  70.00   0.50    0.05    --  113.25 -77.00 120.00   52
 41  ω     42.00  70.00   0.50    0.05    --  113.25 -61.00  30.00   56
 42  ω     42.00  68.00   0.50    0.05    --  113.25 -61.00  60.00   52
 43  ω     46.00  71.00   0.50    0.05    --  113.25 -61.00 -30.00   50
 44  ω     42.00  67.00   0.50    0.05    --  113.25 -61.00 -60.00   50
 45  ω     45.00  71.00   0.50    0.05    --  113.25 -61.00-120.00   52
 46  ω    112.00 161.00   0.50    0.05    --  113.25 113.00 -85.00   98
 47  ω    -63.00  23.00   0.50    0.05    --  -48.02  57.00-150.00  172
 48  ω    -47.00 -19.00   0.50    0.05    --  -91.75 113.00 -85.00   56
 49  ω    -33.00  -7.00   0.50    0.05    --  -48.02 113.00 -85.00   52
 50  ω    -82.00 -43.00   0.50    0.05    --  -48.02 113.00 -85.00   78
 51  ω    -56.00 -12.00   0.50    0.05    --  -48.02  57.00 -60.00   88
 52  ω     -8.00  20.00   0.50    0.05    --  -48.02  57.00 -60.00   56
 53  ω    -49.00 -24.00   0.50    0.05    --  -91.75  45.00   0.00   50
 54  ω    -51.00 -26.00   0.50    0.05    --  -91.75  45.00 150.00   50
 55  ω    -48.00 -20.00   0.50    0.05    --  -91.75  45.00-150.00   56
 56  ω   -161.00 -79.00   0.50    0.05    --  -91.75 -30.00-120.00  164
 57  ω    -63.00 -27.00   0.50    0.05    --  -48.02 -77.00  90.00   72
 58  ω   -119.00 -91.00   0.50    0.05    --  -48.02 -77.00  90.00   56
 59  ω   -114.00 -84.00   0.50    0.05    --  -48.02-125.00   0.00   60
 60  ω   -120.00 -95.00   0.50    0.05    --  -48.02-125.00 -30.00   50
 61  ω   -101.00 -73.00   0.50    0.05    --  -48.02-125.00-150.00   56
 62  ω   -111.00 -85.00   0.50    0.05    --  -91.75-113.00-176.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1431202000
_diffrn_orient_matrix_UB_12      -0.0814471000
_diffrn_orient_matrix_UB_13      -0.0864133000
_diffrn_orient_matrix_UB_21      0.0386801000
_diffrn_orient_matrix_UB_22      0.0315457000
_diffrn_orient_matrix_UB_23      -0.0983194000
_diffrn_orient_matrix_UB_31      0.0511467000
_diffrn_orient_matrix_UB_32      -0.1275135000
_diffrn_orient_matrix_UB_33      -0.0257796000
_diffrn_oxdiff_digest_frames     
;
01a044f0fd73342bcc4865e384e96ff298042784e87
;
_diffrn_oxdiff_digest_hkl        
;
01d69c7dd92c417b09bc5ce8fd313b25ff3252
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4949
_reflns_number_total             5531
_reflns_odcompleteness_completeness 99.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.063
_refine_diff_density_min         -2.045
_refine_diff_density_rms         0.303
_refine_ls_extinction_coef       0.0016(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5531
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0634
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1315P)²+0.0170P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.1820
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H6A(0.049) H6B(0.049) H6(0.029) H7(0.028) H12(0.05) H3(0.035)
 H14A(0.049) H14B(0.049) H14C(0.049) H4(0.034) H13(0.036) H3A(0.07) H10(0.045)
 H11(0.067) H15A(0.08) H15B(0.08) H15C(0.08) H17A(0.103) H17B(0.103) H17C(0.103)
 Fixed X: O11(1) H6A(0.64096) H6B(0.760188) H6(0.318353) H7(0.404503)
 H12(0.844415) H3(0.706732) H14A(0.138381) H14B(0.11845) H14C(0.197132)
 H4(0.528455) H13(0.841973) H3A(0.481824) H10(0.475214) H11(0.654803)
 H15A(0.28384) H15B(0.272355) H15C(0.403856) H17A(0.043088) H17B(0.053905)
 H17C(0.066837)
 Fixed Y: O11(1) H6A(0.671281) H6B(0.771894) H6(0.454304) H7(0.397213)
 H12(0.282406) H3(0.80666) H14A(0.514244) H14B(0.490669) H14C(0.403175)
 H4(0.763909) H13(0.404144) H3A(0.050493) H10(0.162773) H11(0.10393) H15A(-
 0.256877) H15B(-0.113152) H15C(-0.12553) H17A(-0.127116) H17B(-0.250087) H17C(-
 0.260289)
 Fixed Z: O11(0.5) H6A(0.566791) H6B(0.62066) H6(0.79826) H7(0.645255)
 H12(0.229776) H3(1.030918) H14A(0.862586) H14B(0.97501) H14C(0.906056)
 H4(1.099409) H13(0.406384) H3A(0.165894) H10(0.342105) H11(0.101397)
 H15A(0.21536) H15B(0.286389) H15C(0.250595) H17A(0.058251) H17B(0.103459)
 H17C(-0.019672)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo4 Mo 1.03092(5) 1.23137(4) 0.57464(4) 0.02141(18) Uani 1 1 d . . . . .
Mo1 Mo 0.80642(5) 0.57985(5) 0.73882(4) 0.02396(19) Uani 1 1 d D . . . .
Mo2 Mo 1.04996(5) 0.99346(4) 0.68601(4) 0.02200(18) Uani 1 1 d . . . . .
Mo3 Mo 1.22839(5) 1.03237(5) 0.52230(4) 0.02300(19) Uani 1 1 d . . . . .
O12 O 1.0645(5) 1.1745(4) 0.7142(4) 0.0269(9) Uani 1 1 d . . . . .
O15 O 1.2090(5) 1.2157(4) 0.5850(4) 0.0256(9) Uani 1 1 d . . . . .
O10 O 1.2259(5) 1.0141(4) 0.6649(4) 0.0269(9) Uani 1 1 d . . . . .
O13 O 1.1592(5) 0.8422(4) 0.4484(4) 0.0248(9) Uani 1 1 d . . . . .
O11 O 1.000000 1.000000 0.500000 0.0188(11) Uani 1 2 d S T P . .
O8 O 0.8555(5) 0.9532(5) 0.6289(4) 0.0278(9) Uani 1 1 d . . . . .
O2 O 0.7843(5) 0.4599(5) 0.5767(4) 0.0278(9) Uani 1 1 d . . . . .
O5 O 0.3054(5) 0.5896(5) 1.0017(4) 0.0330(10) Uani 1 1 d . . . . .
O1 O 0.7303(5) 0.6821(5) 0.8434(4) 0.0338(10) Uani 1 1 d . . . . .
O9 O 1.0904(6) 0.9816(5) 0.8177(4) 0.0326(10) Uani 1 1 d . . . . .
O16 O 0.9827(5) 1.1976(4) 0.4168(4) 0.0291(10) Uani 1 1 d . . . . .
O4 O 0.9564(5) 0.6879(5) 0.7627(4) 0.0309(10) Uani 1 1 d . . . . .
O17 O 1.0550(5) 1.3987(4) 0.6344(4) 0.0292(10) Uani 1 1 d . . . . .
O14 O 1.3940(5) 1.0625(6) 0.5367(5) 0.0375(11) Uani 1 1 d . . . . .
O6 O 0.7138(5) 0.7029(5) 0.6284(4) 0.0324(10) Uani 1 1 d . . . . .
H6A H 0.640960 0.671281 0.566791 0.049 Uiso 1 1 d DG . . . .
H6B H 0.760188 0.771894 0.620660 0.049 Uiso 1 1 d DG . . . .
N2 N 0.5555(5) 0.3742(5) 0.5357(4) 0.0227(10) Uani 1 1 d . . . . .
N1 N 0.5868(5) 0.4611(5) 0.6480(4) 0.0224(10) Uani 1 1 d . . . . .
O3 O 0.8494(5) 0.4705(5) 0.8054(4) 0.0366(11) Uani 1 1 d . . . . .
O7 O 0.3040(7) -0.0840(7) 0.0727(6) 0.0550(15) Uani 1 1 d . . . . .
C1 C 0.5079(6) 0.5462(6) 0.8065(5) 0.0208(11) Uani 1 1 d . . . . .
C8 C 0.6658(7) 0.3800(6) 0.5080(5) 0.0249(12) Uani 1 1 d . . . . .
C6 C 0.3979(6) 0.5248(6) 0.8460(5) 0.0240(12) Uani 1 1 d . . . . .
H6 H 0.318353 0.454304 0.798260 0.029 Uiso 1 1 calc R . . . .
C5 C 0.4050(7) 0.6058(6) 0.9538(5) 0.0248(12) Uani 1 1 d . . . . .
C9 C 0.6608(7) 0.2981(6) 0.3938(5) 0.0248(12) Uani 1 1 d . . . . .
C7 C 0.4907(6) 0.4589(6) 0.6912(5) 0.0231(11) Uani 1 1 d . . . . .
H7 H 0.404503 0.397213 0.645255 0.028 Uiso 1 1 calc R . . . .
C12 C 0.7682(10) 0.2594(8) 0.2519(7) 0.042(2) Uani 1 1 d . . . . .
H12 H 0.844415 0.282406 0.229776 0.050 Uiso 1 1 calc R . . . .
C2 C 0.6231(6) 0.6517(6) 0.8766(5) 0.0230(12) Uani 1 1 d . . . . .
C3 C 0.6289(7) 0.7337(6) 0.9843(5) 0.0291(13) Uani 1 1 d . . . . .
H3 H 0.706732 0.806660 1.030918 0.035 Uiso 1 1 calc R . . . .
C14 C 0.1801(7) 0.4918(8) 0.9308(6) 0.0329(14) Uani 1 1 d . . . . .
H14A H 0.138381 0.514244 0.862586 0.049 Uiso 1 1 calc GR . . . .
H14B H 0.118450 0.490669 0.975010 0.049 Uiso 1 1 calc GR . . . .
H14C H 0.197132 0.403175 0.906056 0.049 Uiso 1 1 calc GR . . . .
C4 C 0.5221(7) 0.7098(7) 1.0244(5) 0.0284(13) Uani 1 1 d . . . . .
H4 H 0.528455 0.763909 1.099409 0.034 Uiso 1 1 calc R . . . .
C13 C 0.7668(8) 0.3298(6) 0.3565(6) 0.0302(14) Uani 1 1 d . . . . .
H13 H 0.841973 0.404144 0.406384 0.036 Uiso 1 1 calc R . . . .
N3 N 0.5514(9) 0.1192(8) 0.2128(6) 0.058(2) Uani 1 1 d . . . . .
H3A H 0.481824 0.050493 0.165894 0.070 Uiso 1 1 calc R . . . .
C10 C 0.5499(8) 0.1883(7) 0.3189(6) 0.0373(16) Uani 1 1 d . . . . .
H10 H 0.475214 0.162773 0.342105 0.045 Uiso 1 1 calc R . . . .
C16 C 0.2376(8) -0.1425(8) 0.1163(6) 0.0420(17) Uani 1 1 d . . . . .
C11 C 0.6571(12) 0.1526(10) 0.1766(7) 0.056(3) Uani 1 1 d . . . . .
H11 H 0.654803 0.103930 0.101397 0.067 Uiso 1 1 calc R . . . .
C15 C 0.3051(12) -0.1611(9) 0.2265(7) 0.053(2) Uani 1 1 d . . . . .
H15A H 0.283840 -0.256877 0.215360 0.080 Uiso 1 1 calc GR . . . .
H15B H 0.272355 -0.113152 0.286389 0.080 Uiso 1 1 calc GR . . . .
H15C H 0.403856 -0.125530 0.250595 0.080 Uiso 1 1 calc GR . . . .
C17 C 0.0875(11) -0.1999(13) 0.0597(9) 0.069(3) Uani 1 1 d . . . . .
H17A H 0.043088 -0.127116 0.058251 0.103 Uiso 1 1 calc GR . . . .
H17B H 0.053905 -0.250087 0.103459 0.103 Uiso 1 1 calc GR . . . .
H17C H 0.066837 -0.260289 -0.019672 0.103 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo4 O12 2.015(4) . ?
Mo4 O15 1.895(5) . ?
Mo4 O13 1.949(5) 2_776 ?
Mo4 O11 2.3321(4) . ?
Mo4 O16 1.855(5) . ?
Mo4 O17 1.690(4) . ?
Mo1 O2 2.037(4) . ?
Mo1 O1 1.928(5) . ?
Mo1 O4 1.705(5) . ?
Mo1 O6 2.335(5) . ?
Mo1 N1 2.255(5) . ?
Mo1 O3 1.691(5) . ?
Mo2 O12 1.853(4) . ?
Mo2 O10 1.947(5) . ?
Mo2 O11 2.3223(4) . ?
Mo2 O8 1.914(5) . ?
Mo2 O9 1.673(5) . ?
Mo2 O16 2.015(4) 2_776 ?
Mo3 O15 1.977(4) . ?
Mo3 O10 1.905(5) . ?
Mo3 O13 1.912(4) . ?
Mo3 O11 2.3140(5) . ?
Mo3 O8 1.959(5) 2_776 ?
Mo3 O14 1.681(5) . ?
O2 C8 1.302(8) . ?
O5 C5 1.376(8) . ?
O5 C14 1.424(9) . ?
O1 C2 1.348(8) . ?
O6 H6A 0.8699 . ?
O6 H6B 0.8703 . ?
N2 N1 1.387(6) . ?
N2 C8 1.313(8) . ?
N1 C7 1.291(8) . ?
O7 C16 1.221(11) . ?
C1 C6 1.410(9) . ?
C1 C7 1.452(7) . ?
C1 C2 1.395(9) . ?
C8 C9 1.461(8) . ?
C6 H6 0.9500 . ?
C6 C5 1.383(8) . ?
C5 C4 1.400(9) . ?
C9 C13 1.373(9) . ?
C9 C10 1.405(9) . ?
C7 H7 0.9500 . ?
C12 H12 0.9500 . ?
C12 C13 1.346(9) . ?
C12 C11 1.391(15) . ?
C2 C3 1.390(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(10) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C4 H4 0.9500 . ?
C13 H13 0.9500 . ?
N3 H3A 0.8800 . ?
N3 C10 1.359(10) . ?
N3 C11 1.366(15) . ?
C10 H10 0.9500 . ?
C16 C15 1.482(12) . ?
C16 C17 1.490(13) . ?
C11 H11 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O12 Mo4 O11 75.48(12) . . ?
O15 Mo4 O12 84.7(2) . . ?
O15 Mo4 O13 152.68(18) . 2_776 ?
O15 Mo4 O11 77.03(13) . . ?
O13 Mo4 O12 82.9(2) 2_776 . ?
O13 Mo4 O11 76.34(12) 2_776 . ?
O16 Mo4 O12 153.13(18) . . ?
O16 Mo4 O15 91.1(2) . . ?
O16 Mo4 O13 89.2(2) . 2_776 ?
O16 Mo4 O11 77.71(13) . . ?
O17 Mo4 O12 102.08(19) . . ?
O17 Mo4 O15 102.8(2) . . ?
O17 Mo4 O13 103.6(2) . 2_776 ?
O17 Mo4 O11 177.56(15) . . ?
O17 Mo4 O16 104.7(2) . . ?
O2 Mo1 O6 78.95(19) . . ?
O2 Mo1 N1 71.44(18) . . ?
O1 Mo1 O2 149.6(2) . . ?
O1 Mo1 O6 81.3(2) . . ?
O1 Mo1 N1 81.7(2) . . ?
O4 Mo1 O2 96.3(2) . . ?
O4 Mo1 O1 104.0(2) . . ?
O4 Mo1 O6 83.2(2) . . ?
O4 Mo1 N1 158.1(2) . . ?
N1 Mo1 O6 76.71(18) . . ?
O3 Mo1 O2 96.3(2) . . ?
O3 Mo1 O1 99.6(2) . . ?
O3 Mo1 O4 105.6(3) . . ?
O3 Mo1 O6 170.5(2) . . ?
O3 Mo1 N1 94.0(2) . . ?
O12 Mo2 O10 90.2(2) . . ?
O12 Mo2 O11 78.72(13) . . ?
O12 Mo2 O8 91.3(2) . . ?
O12 Mo2 O16 153.75(18) . 2_776 ?
O10 Mo2 O11 76.63(13) . . ?
O10 Mo2 O16 83.1(2) . 2_776 ?
O8 Mo2 O10 152.46(19) . . ?
O8 Mo2 O11 76.71(14) . . ?
O8 Mo2 O16 83.5(2) . 2_776 ?
O9 Mo2 O12 104.0(2) . . ?
O9 Mo2 O10 101.3(2) . . ?
O9 Mo2 O11 176.63(17) . . ?
O9 Mo2 O8 105.0(2) . . ?
O9 Mo2 O16 102.2(2) . 2_776 ?
O16 Mo2 O11 75.04(13) 2_776 . ?
O15 Mo3 O11 75.97(13) . . ?
O10 Mo3 O15 86.74(19) . . ?
O10 Mo3 O13 89.27(19) . . ?
O10 Mo3 O11 77.62(14) . . ?
O10 Mo3 O8 153.6(2) . 2_776 ?
O13 Mo3 O15 153.40(19) . . ?
O13 Mo3 O11 77.49(13) . . ?
O13 Mo3 O8 87.47(19) . 2_776 ?
O8 Mo3 O15 84.57(19) 2_776 . ?
O8 Mo3 O11 76.09(14) 2_776 . ?
O14 Mo3 O15 101.9(2) . . ?
O14 Mo3 O10 104.1(2) . . ?
O14 Mo3 O13 104.6(2) . . ?
O14 Mo3 O11 177.2(2) . . ?
O14 Mo3 O8 102.1(2) . 2_776 ?
Mo2 O12 Mo4 116.1(2) . . ?
Mo4 O15 Mo3 116.6(2) . . ?
Mo3 O10 Mo2 116.0(2) . . ?
Mo3 O13 Mo4 116.1(2) . 2_776 ?
Mo4 O11 Mo4 180.00(3) 2_776 . ?
Mo2 O11 Mo4 89.703(16) . . ?
Mo2 O11 Mo4 89.703(17) 2_776 2_776 ?
Mo2 O11 Mo4 90.297(16) 2_776 . ?
Mo2 O11 Mo4 90.296(16) . 2_776 ?
Mo2 O11 Mo2 180.0 . 2_776 ?
Mo3 O11 Mo4 90.301(18) 2_776 2_776 ?
Mo3 O11 Mo4 89.698(18) 2_776 . ?
Mo3 O11 Mo4 89.698(17) . 2_776 ?
Mo3 O11 Mo4 90.302(17) . . ?
Mo3 O11 Mo2 90.380(18) . 2_776 ?
Mo3 O11 Mo2 89.619(18) . . ?
Mo3 O11 Mo2 90.381(18) 2_776 . ?
Mo3 O11 Mo2 89.620(18) 2_776 2_776 ?
Mo3 O11 Mo3 180.0 . 2_776 ?
Mo2 O8 Mo3 116.3(2) . 2_776 ?
C8 O2 Mo1 119.8(4) . . ?
C5 O5 C14 117.7(5) . . ?
C2 O1 Mo1 134.1(4) . . ?
Mo4 O16 Mo2 116.9(2) . 2_776 ?
Mo1 O6 H6A 125.3 . . ?
Mo1 O6 H6B 125.0 . . ?
H6A O6 H6B 104.5 . . ?
C8 N2 N1 109.9(5) . . ?
N2 N1 Mo1 115.4(4) . . ?
C7 N1 Mo1 127.3(4) . . ?
C7 N1 N2 117.1(5) . . ?
C6 C1 C7 116.9(5) . . ?
C2 C1 C6 119.1(5) . . ?
C2 C1 C7 123.9(6) . . ?
O2 C8 N2 123.5(5) . . ?
O2 C8 C9 115.5(6) . . ?
N2 C8 C9 121.0(6) . . ?
C1 C6 H6 119.7 . . ?
C5 C6 C1 120.5(6) . . ?
C5 C6 H6 119.7 . . ?
O5 C5 C6 124.8(6) . . ?
O5 C5 C4 115.3(5) . . ?
C6 C5 C4 119.9(6) . . ?
C13 C9 C8 119.4(6) . . ?
C13 C9 C10 118.2(6) . . ?
C10 C9 C8 122.4(6) . . ?
N1 C7 C1 123.2(6) . . ?
N1 C7 H7 118.4 . . ?
C1 C7 H7 118.4 . . ?
C13 C12 H12 120.3 . . ?
C13 C12 C11 119.4(8) . . ?
C11 C12 H12 120.3 . . ?
O1 C2 C1 122.8(6) . . ?
O1 C2 C3 117.1(6) . . ?
C3 C2 C1 120.1(6) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.6(6) . . ?
C4 C3 H3 119.7 . . ?
O5 C14 H14A 109.5 . . ?
O5 C14 H14B 109.5 . . ?
O5 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C5 C4 H4 120.1 . . ?
C3 C4 C5 119.8(6) . . ?
C3 C4 H4 120.1 . . ?
C9 C13 H13 118.8 . . ?
C12 C13 C9 122.5(7) . . ?
C12 C13 H13 118.8 . . ?
C10 N3 H3A 118.9 . . ?
C10 N3 C11 122.2(8) . . ?
C11 N3 H3A 118.9 . . ?
C9 C10 H10 120.6 . . ?
N3 C10 C9 118.9(8) . . ?
N3 C10 H10 120.6 . . ?
O7 C16 C15 120.6(8) . . ?
O7 C16 C17 121.5(9) . . ?
C15 C16 C17 117.9(9) . . ?
C12 C11 H11 120.6 . . ?
N3 C11 C12 118.8(7) . . ?
N3 C11 H11 120.6 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O2 C8 N2 2.1(8) . . . . ?
Mo1 O2 C8 C9 -179.9(4) . . . . ?
Mo1 O1 C2 C1 -27.3(9) . . . . ?
Mo1 O1 C2 C3 154.7(5) . . . . ?
Mo1 N1 C7 C1 6.3(8) . . . . ?
O12 Mo4 O15 Mo3 79.3(2) . . . . ?
O12 Mo4 O16 Mo2 -5.5(7) . . . 2_776 ?
O15 Mo4 O16 Mo2 74.8(3) . . . 2_776 ?
O10 Mo2 O12 Mo4 75.7(3) . . . . ?
O13 Mo4 O15 Mo3 16.2(6) 2_776 . . . ?
O13 Mo4 O16 Mo2 -77.9(3) 2_776 . . 2_776 ?
O11 Mo4 O15 Mo3 3.01(18) . . . . ?
O11 Mo4 O16 Mo2 -1.7(2) . . . 2_776 ?
O11 Mo2 O12 Mo4 -0.6(2) . . . . ?
O8 Mo2 O12 Mo4 -76.8(3) . . . . ?
O2 C8 C9 C13 -14.4(8) . . . . ?
O2 C8 C9 C10 166.5(6) . . . . ?
O5 C5 C4 C3 179.5(6) . . . . ?
O1 C2 C3 C4 179.4(6) . . . . ?
O9 Mo2 O12 Mo4 177.4(3) . . . . ?
O16 Mo4 O15 Mo3 -74.1(3) . . . . ?
O16 Mo2 O12 Mo4 0.9(6) 2_776 . . . ?
O17 Mo4 O15 Mo3 -179.5(2) . . . . ?
O17 Mo4 O16 Mo2 178.3(3) . . . 2_776 ?
N2 N1 C7 C1 -178.6(5) . . . . ?
N2 C8 C9 C13 163.5(6) . . . . ?
N2 C8 C9 C10 -15.5(9) . . . . ?
N1 N2 C8 O2 -2.0(8) . . . . ?
N1 N2 C8 C9 -179.8(5) . . . . ?
C1 C6 C5 O5 -177.4(6) . . . . ?
C1 C6 C5 C4 0.0(9) . . . . ?
C1 C2 C3 C4 1.5(9) . . . . ?
C8 N2 N1 Mo1 1.0(6) . . . . ?
C8 N2 N1 C7 -174.6(5) . . . . ?
C8 C9 C13 C12 -179.4(6) . . . . ?
C8 C9 C10 N3 178.4(6) . . . . ?
C6 C1 C7 N1 -174.6(5) . . . . ?
C6 C1 C2 O1 -177.4(5) . . . . ?
C6 C1 C2 C3 0.5(9) . . . . ?
C6 C5 C4 C3 1.9(9) . . . . ?
C7 C1 C6 C5 -178.5(5) . . . . ?
C7 C1 C2 O1 -0.3(9) . . . . ?
C7 C1 C2 C3 177.5(6) . . . . ?
C2 C1 C6 C5 -1.2(8) . . . . ?
C2 C1 C7 N1 8.2(9) . . . . ?
C2 C3 C4 C5 -2.6(10) . . . . ?
C14 O5 C5 C6 -7.0(9) . . . . ?
C14 O5 C5 C4 175.5(6) . . . . ?
C13 C9 C10 N3 -0.7(10) . . . . ?
C13 C12 C11 N3 -2.4(10) . . . . ?
C10 C9 C13 C12 -0.3(9) . . . . ?
C10 N3 C11 C12 1.4(12) . . . . ?
C11 C12 C13 C9 1.8(10) . . . . ?
C11 N3 C10 C9 0.2(11) . . . . ?

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.752
_oxdiff_exptl_absorpt_empirical_full_min 0.476
# start Validation Reply Form
_vrf_PLAT973_exp_2115_auto       
;
PROBLEM: Check Calcd Positive Resid. Density on       Mo1       1.92 eA-3  
RESPONSE: Artifact due to insufficient data quality.
;
_vrf_PLAT976_exp_2115_auto       
;
PROBLEM: Check Calcd Resid. Dens.  1.03Ang From O10     .      -1.55 eA-3  
RESPONSE: Artifact due to insufficient data quality.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3H
_database_code_depnum_ccdc_archive 'CCDC 2335836'
loop_
_audit_author_name
_audit_author_address
'Mirta Rubcic'
;University of Zagreb
Croatia
;
_audit_update_record             
;
2024-02-27 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-05-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Mo6 O19, 2(C14 H12 Mo N3 O5)'
_chemical_formula_sum            'C28 H24 Mo8 N6 O29'
_chemical_formula_weight         1676.05
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Mo4 N3 O14 C13'
_chemical_oxdiff_usercomment     ' '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8403(2)
_cell_length_b                   9.1695(2)
_cell_length_c                   14.0494(3)
_cell_angle_alpha                106.381(2)
_cell_angle_beta                 105.966(2)
_cell_angle_gamma                93.753(2)
_cell_volume                     1037.78(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    8579
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      77.2400
_cell_measurement_theta_min      3.4170
_shelx_estimated_absorpt_T_max   0.665
_shelx_estimated_absorpt_T_min   0.245
_exptl_absorpt_coefficient_mu    20.157
_exptl_absorpt_correction_T_max  0.04313
_exptl_absorpt_correction_T_min  0.00166
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'grayish red'
_exptl_crystal_colour_lustre     ?
_exptl_crystal_colour_modifier   grayish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.682
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       sphere
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.022
_exptl_crystal_size_rad          0.400
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14341
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.001
_diffrn_reflns_theta_min         5.089
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    101.00 162.00   0.50    0.09    --  107.75  30.00   0.00  122
  2  ω     94.00 169.00   0.50    0.09    --  107.75  15.00  60.00  150
  3  ω     96.00 166.00   0.50    0.09    --  107.75  15.00 120.00  140
  4  ω     97.00 178.00   0.50    0.09    --  107.75  15.00 -30.00  162
  5  ω    106.00 131.00   0.50    0.09    --  107.75  15.00-180.00   50
  6  ω    141.00 177.00   0.50    0.09    --  107.75  15.00-180.00   72
  7  ω    100.00 176.00   0.50    0.09    --  107.75  30.00-120.00  152
  8  ω     73.00  98.00   0.50    0.09    --  107.75 -95.00  90.00   50
  9  ω     55.00 112.00   0.50    0.09    --  107.75-125.00  90.00  114
 10  ω     87.00 112.00   0.50    0.09    --  107.75-125.00  60.00   50
 11  ω     60.00  86.00   0.50    0.09    --  107.75-125.00  60.00   52
 12  ω     44.00 107.00   0.50    0.09    --  107.75-102.00  22.68  126
 13  ω     71.00 101.00   0.50    0.09    --  107.75 -96.00 137.00   60
 14  ω     -4.00  78.00   0.50    0.05    --   46.91 -96.00 137.00  164
 15  ω     46.00 101.00   0.50    0.09    --  107.75 -95.00 120.00  110
 16  ω     44.00 112.00   0.50    0.09    --  107.75-125.00 -60.00  136
 17  ω     73.00  99.00   0.50    0.09    --  107.75 -95.00-180.00   52
 18  ω     87.00 112.00   0.50    0.09    --  107.75-125.00-150.00   50
 19  ω     77.00 108.00   0.50    0.09    --  107.75-109.00 -66.79   62
 20  ω     60.00 104.00   0.50    0.09    --  107.75 -95.00 -60.00   88
 21  ω     36.00  91.00   0.50    0.09    --  107.75 -95.00 -30.00  110
 22  ω     38.00  69.00   0.50    0.09    --  107.75 -95.00  60.00   62
 23  ω     44.00  69.00   0.50    0.09    --  107.75 -95.00  90.00   50
 24  ω     77.00 103.00   0.50    0.09    --  107.75 -95.00  60.00   52
 25  ω     35.00  70.00   0.50    0.09    --  107.75 -95.00-180.00   70
 26  ω     62.00 104.00   0.50    0.09    --  107.75 -77.00 -60.00   84
 27  ω     42.00  73.00   0.50    0.09    --  107.75 -77.00-180.00   62
 28  ω     60.00  86.00   0.50    0.09    --  107.75 -77.00-150.00   52
 29  ω     36.00  71.00   0.50    0.09    --  107.75 -61.00-180.00   70
 30  ω     39.00  70.00   0.50    0.09    --  107.75 -77.00 -90.00   62
 31  ω    -19.00  25.00   0.50    0.05    --   46.91 -19.00-150.00   88
 32  ω     37.00  63.00   0.50    0.09    --  107.75 -77.00  60.00   52
 33  ω     46.00  87.00   0.50    0.09    --  107.75 -77.00  90.00   82
 34  ω     35.00  68.00   0.50    0.09    --  107.75 -61.00 120.00   66
 35  ω    117.00 165.00   0.50    0.09    --  107.75  96.00-114.00   96
 36  ω     98.00 123.00   0.50    0.09    --  107.75 125.00   0.00   50
 37  ω    115.00 140.00   0.50    0.09    --  107.75 125.00 -30.00   50
 38  ω    133.00 159.00   0.50    0.09    --  107.75 125.00   0.00   52
 39  ω    -43.00  -7.00   0.50    0.05    --  -46.91  38.00-150.00   72
 40  ω     -3.00  24.00   0.50    0.05    --  -46.91  38.00-150.00   54
 41  ω    -47.00 -14.00   0.50    0.09    --  -86.25  45.00 -90.00   66
 42  ω    -50.00 -14.00   0.50    0.09    --  -86.25  45.00  30.00   72
 43  ω    -50.00 -24.00   0.50    0.09    --  -86.25  45.00  90.00   52
 44  ω   -158.00-113.00   0.50    0.09    --  -86.25 -45.00 -30.00   90
 45  ω   -118.00 -78.00   0.50    0.05    --  -46.91-125.00 -60.00   80
 46  ω   -117.00 -73.00   0.50    0.05    --  -46.91-125.00-120.00   88
 47  ω   -118.00 -74.00   0.50    0.05    --  -46.91-125.00-150.00   88
 48  ω   -146.00-121.00   0.50    0.09    --  -86.25 -96.00 137.00   50
 49  ω    -53.00  25.00   0.50    0.05    --  -46.91  96.00-114.00  156
 50  ω    -71.00 -46.00   0.50    0.09    --  -86.25  96.00-114.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0042145000
_diffrn_orient_matrix_UB_12      -0.0083344000
_diffrn_orient_matrix_UB_13      -0.1102849000
_diffrn_orient_matrix_UB_21      0.0195869000
_diffrn_orient_matrix_UB_22      -0.1709326000
_diffrn_orient_matrix_UB_23      -0.0222202000
_diffrn_orient_matrix_UB_31      -0.1823794000
_diffrn_orient_matrix_UB_32      -0.0462017000
_diffrn_orient_matrix_UB_33      -0.0419713000
_diffrn_oxdiff_digest_frames     
;
01f90d87c4acf4f94707412155742f9f8f00065f6f2
;
_diffrn_oxdiff_digest_hkl        
;
01225711ddc4f5e35f1d9ccd0135025aeb3cd5
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4083
_reflns_number_total             4320
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         2.554
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.473
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4320
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0802
_refine_ls_restrained_S_all      1.172
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1417P)²+0.3354P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1975
_refine_ls_wR_factor_ref         0.2002
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H3(0.068) H6(0.062) H12(0.073) H4(0.065) H3A(0.063) H13(0.067)
 H10(0.064) H14A(0.087) H14B(0.087) H14C(0.087) H11(0.076) H7(0.06)
 Fixed X: O9(0.5) H3(0.843001) H6(0.034671) H12(1.166743) H4(-0.099069)
 H3A(0.14621) H13(0.985487) H10(0.667946) H14A(-0.297274) H14B(-0.420762) H14C(-
 0.35138) H11(1.085859) H7(0.28176)
 Fixed Y: O9(0.5) H3(1.090816) H6(0.433785) H12(0.862807) H4(-0.030336) H3A(-
 0.050136) H13(0.631501) H10(0.878854) H14A(0.0213) H14B(0.14042)
 H14C(0.069816) H11(1.094625) H7(0.558578)
 Fixed Z: O9(1) H3(0.815363) H6(0.422509) H12(0.933974) H4(0.338511)
 H3A(0.44557) H13(0.837997) H10(0.719719) H14A(0.218156) H14B(0.228832)
 H14C(0.321029) H11(0.91723) H7(0.552819)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo2 Mo 0.32195(6) 0.40677(6) 0.83043(4) 0.0481(2) Uani 1 1 d . . . . .
Mo3 Mo 0.29328(6) 0.58948(6) 1.06077(4) 0.0482(2) Uani 1 1 d . . . . .
Mo4 Mo 0.55683(6) 0.73232(6) 0.97446(5) 0.0489(2) Uani 1 1 d . . . . .
Mo1 Mo 0.58488(6) 0.26310(6) 0.62482(5) 0.0501(2) Uani 1 1 d . . . . .
O9 O 0.500000 0.500000 1.000000 0.0478(14) Uani 1 2 d S T P . .
O8 O 0.2947(6) 0.2456(6) 0.8803(4) 0.0540(11) Uani 1 1 d . . . . .
O2 O 0.7376(6) 0.4587(6) 0.7118(4) 0.0514(11) Uani 1 1 d . . . . .
O12 O 0.1981(6) 0.5197(6) 0.9162(4) 0.0517(11) Uani 1 1 d . . . . .
O10 O 0.4110(6) 0.6277(6) 0.8494(4) 0.0498(10) Uani 1 1 d . . . . .
O13 O 0.3985(6) 0.7682(6) 1.0428(4) 0.0531(11) Uani 1 1 d . . . . .
O4 O 0.6730(6) 0.1473(6) 0.6928(5) 0.0550(11) Uani 1 1 d . . . . .
O14 O 0.2806(6) 0.3877(6) 1.0670(4) 0.0489(10) Uani 1 1 d . . . . .
O6 O 0.5184(6) 0.3596(6) 0.8073(4) 0.0488(10) Uani 1 1 d . . . . .
O5 O -0.1971(6) 0.2310(6) 0.3138(5) 0.0558(12) Uani 1 1 d . . . . .
O1 O 0.3694(6) 0.1618(6) 0.5704(5) 0.0567(12) Uani 1 1 d . . . . .
O11 O 0.6164(7) 0.9025(6) 0.9614(5) 0.0560(12) Uani 1 1 d . . . . .
O3 O 0.6453(7) 0.2297(7) 0.5176(5) 0.0622(13) Uani 1 1 d . . . . .
O15 O 0.1466(6) 0.6638(7) 1.1037(4) 0.0541(11) Uani 1 1 d . . . . .
O7 O 0.1869(6) 0.3518(7) 0.7102(4) 0.0576(12) Uani 1 1 d . . . . .
N3 N 0.8713(8) 1.0020(8) 0.8194(6) 0.0564(14) Uani 1 1 d . . . . .
H3 H 0.843001 1.090816 0.815363 0.068 Uiso 1 1 calc R . . . .
N2 N 0.5491(7) 0.6074(7) 0.6611(5) 0.0500(12) Uani 1 1 d . . . . .
N1 N 0.4592(7) 0.4623(7) 0.6093(5) 0.0490(12) Uani 1 1 d . . . . .
C9 C 0.8083(9) 0.7319(8) 0.7725(6) 0.0496(14) Uani 1 1 d . . . . .
C5 C -0.0578(8) 0.2042(8) 0.3720(6) 0.0503(14) Uani 1 1 d . . . . .
C2 C 0.2361(8) 0.1766(9) 0.5014(6) 0.0521(15) Uani 1 1 d . . . . .
C6 C 0.0569(8) 0.3361(9) 0.4284(6) 0.0516(14) Uani 1 1 d . . . . .
H6 H 0.034671 0.433785 0.422509 0.062 Uiso 1 1 calc R . . . .
C1 C 0.2049(8) 0.3233(8) 0.4936(6) 0.0482(14) Uani 1 1 d . . . . .
C12 C 1.0639(9) 0.8644(11) 0.8903(6) 0.0612(19) Uani 1 1 d . . . . .
H12 H 1.166743 0.862807 0.933974 0.073 Uiso 1 1 calc R . . . .
C8 C 0.6905(8) 0.5917(9) 0.7103(6) 0.0498(14) Uani 1 1 d . . . . .
C4 C -0.0230(9) 0.0594(9) 0.3781(6) 0.0539(15) Uani 1 1 d . . . . .
H4 H -0.099069 -0.030336 0.338511 0.065 Uiso 1 1 calc R . . . .
C3 C 0.1231(8) 0.0483(9) 0.4422(6) 0.0522(15) Uani 1 1 d . . . . .
H3A H 0.146210 -0.050136 0.445570 0.063 Uiso 1 1 calc R . . . .
C13 C 0.9554(9) 0.7275(10) 0.8335(6) 0.0557(16) Uani 1 1 d . . . . .
H13 H 0.985487 0.631501 0.837997 0.067 Uiso 1 1 calc R . . . .
C10 C 0.7686(9) 0.8739(9) 0.7645(7) 0.0530(15) Uani 1 1 d . . . . .
H10 H 0.667946 0.878854 0.719719 0.064 Uiso 1 1 calc R . . . .
C14 C -0.3269(9) 0.1057(9) 0.2667(7) 0.0580(17) Uani 1 1 d . . . . .
H14A H -0.297274 0.021300 0.218156 0.087 Uiso 1 1 calc GR . . . .
H14B H -0.420762 0.140420 0.228832 0.087 Uiso 1 1 calc GR . . . .
H14C H -0.351380 0.069816 0.321029 0.087 Uiso 1 1 calc GR . . . .
C11 C 1.0153(11) 1.0005(11) 0.8802(7) 0.0631(19) Uani 1 1 d . . . . .
H11 H 1.085859 1.094625 0.917230 0.076 Uiso 1 1 calc R . . . .
C7 C 0.3155(8) 0.4626(8) 0.5538(6) 0.0497(14) Uani 1 1 d . . . . .
H7 H 0.281760 0.558578 0.552819 0.060 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo2 O9 2.3444(5) . ?
Mo2 O8 1.834(6) . ?
Mo2 O12 1.973(5) . ?
Mo2 O10 2.042(5) . ?
Mo2 O6 1.908(5) . ?
Mo2 O7 1.693(5) . ?
Mo3 O9 2.3241(5) . ?
Mo3 O12 1.870(5) . ?
Mo3 O13 1.943(5) . ?
Mo3 O14 1.874(5) . ?
Mo3 O6 2.034(5) 2_667 ?
Mo3 O15 1.681(5) . ?
Mo4 O9 2.3042(5) . ?
Mo4 O8 2.046(6) 2_667 ?
Mo4 O10 1.820(5) . ?
Mo4 O13 1.901(6) . ?
Mo4 O14 1.981(5) 2_667 ?
Mo4 O11 1.689(5) . ?
Mo1 O2 2.018(5) . ?
Mo1 O4 1.708(6) . ?
Mo1 O1 1.909(5) . ?
Mo1 O3 1.689(6) . ?
Mo1 N1 2.230(6) . ?
O2 C8 1.318(9) . ?
O5 C5 1.358(9) . ?
O5 C14 1.433(9) . ?
O1 C2 1.346(9) . ?
N3 H3 0.8800 . ?
N3 C10 1.328(10) . ?
N3 C11 1.326(12) . ?
N2 N1 1.389(8) . ?
N2 C8 1.290(10) . ?
N1 C7 1.295(10) . ?
C9 C8 1.480(10) . ?
C9 C13 1.356(11) . ?
C9 C10 1.398(11) . ?
C5 C6 1.405(10) . ?
C5 C4 1.403(11) . ?
C2 C1 1.419(11) . ?
C2 C3 1.382(10) . ?
C6 H6 0.9500 . ?
C6 C1 1.410(10) . ?
C1 C7 1.441(10) . ?
C12 H12 0.9500 . ?
C12 C13 1.410(11) . ?
C12 C11 1.379(14) . ?
C4 H4 0.9500 . ?
C4 C3 1.385(11) . ?
C3 H3A 0.9500 . ?
C13 H13 0.9500 . ?
C10 H10 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C11 H11 0.9500 . ?
C7 H7 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 Mo2 O9 78.31(17) . . ?
O8 Mo2 O12 88.8(2) . . ?
O8 Mo2 O10 152.2(2) . . ?
O8 Mo2 O6 94.1(2) . . ?
O12 Mo2 O9 75.00(15) . . ?
O12 Mo2 O10 80.0(2) . . ?
O10 Mo2 O9 74.29(15) . . ?
O6 Mo2 O9 78.27(15) . . ?
O6 Mo2 O12 151.9(2) . . ?
O6 Mo2 O10 84.7(2) . . ?
O7 Mo2 O9 175.6(2) . . ?
O7 Mo2 O8 104.2(3) . . ?
O7 Mo2 O12 101.3(3) . . ?
O7 Mo2 O10 102.9(3) . . ?
O7 Mo2 O6 105.0(3) . . ?
O12 Mo3 O9 77.35(16) . . ?
O12 Mo3 O13 87.4(2) . . ?
O12 Mo3 O14 91.5(2) . . ?
O12 Mo3 O6 153.6(2) . 2_667 ?
O13 Mo3 O9 75.83(17) . . ?
O13 Mo3 O6 83.4(2) . 2_667 ?
O14 Mo3 O9 77.31(16) . . ?
O14 Mo3 O13 152.7(2) . . ?
O14 Mo3 O6 85.6(2) . 2_667 ?
O6 Mo3 O9 76.41(14) 2_667 . ?
O15 Mo3 O9 176.7(2) . . ?
O15 Mo3 O12 102.4(3) . . ?
O15 Mo3 O13 100.9(3) . . ?
O15 Mo3 O14 106.0(3) . . ?
O15 Mo3 O6 103.7(2) . 2_667 ?
O8 Mo4 O9 75.39(15) 2_667 . ?
O10 Mo4 O9 79.36(16) . . ?
O10 Mo4 O8 154.6(2) . 2_667 ?
O10 Mo4 O13 92.9(2) . . ?
O10 Mo4 O14 89.9(2) . 2_667 ?
O13 Mo4 O9 77.10(16) . . ?
O13 Mo4 O8 84.5(2) . 2_667 ?
O13 Mo4 O14 151.8(2) . 2_667 ?
O14 Mo4 O9 75.85(14) 2_667 . ?
O14 Mo4 O8 81.2(2) 2_667 2_667 ?
O11 Mo4 O9 174.68(19) . . ?
O11 Mo4 O8 100.4(3) . 2_667 ?
O11 Mo4 O10 104.6(3) . . ?
O11 Mo4 O13 106.0(3) . . ?
O11 Mo4 O14 100.4(2) . 2_667 ?
O2 Mo1 N1 71.7(2) . . ?
O4 Mo1 O2 97.0(2) . . ?
O4 Mo1 O1 101.1(2) . . ?
O4 Mo1 N1 153.3(3) . . ?
O1 Mo1 O2 147.1(2) . . ?
O1 Mo1 N1 80.0(2) . . ?
O3 Mo1 O2 97.7(3) . . ?
O3 Mo1 O4 106.7(3) . . ?
O3 Mo1 O1 103.0(3) . . ?
O3 Mo1 N1 98.9(3) . . ?
Mo2 O9 Mo2 180.0 . 2_667 ?
Mo3 O9 Mo2 90.552(19) . 2_667 ?
Mo3 O9 Mo2 89.448(19) . . ?
Mo3 O9 Mo2 89.447(19) 2_667 2_667 ?
Mo3 O9 Mo2 90.553(19) 2_667 . ?
Mo3 O9 Mo3 180.0 2_667 . ?
Mo4 O9 Mo2 90.10(2) 2_667 . ?
Mo4 O9 Mo2 89.903(19) 2_667 2_667 ?
Mo4 O9 Mo2 90.10(2) . 2_667 ?
Mo4 O9 Mo2 89.903(19) . . ?
Mo4 O9 Mo3 90.24(2) . 2_667 ?
Mo4 O9 Mo3 90.24(2) 2_667 . ?
Mo4 O9 Mo3 89.76(2) 2_667 2_667 ?
Mo4 O9 Mo3 89.75(2) . . ?
Mo4 O9 Mo4 180.0 . 2_667 ?
Mo2 O8 Mo4 115.9(3) . 2_667 ?
C8 O2 Mo1 118.7(4) . . ?
Mo3 O12 Mo2 117.4(3) . . ?
Mo4 O10 Mo2 116.4(3) . . ?
Mo4 O13 Mo3 116.3(3) . . ?
Mo3 O14 Mo4 116.6(2) . 2_667 ?
Mo2 O6 Mo3 114.6(3) . 2_667 ?
C5 O5 C14 117.4(6) . . ?
C2 O1 Mo1 135.3(5) . . ?
C10 N3 H3 118.9 . . ?
C11 N3 H3 118.9 . . ?
C11 N3 C10 122.2(7) . . ?
C8 N2 N1 108.6(6) . . ?
N2 N1 Mo1 116.2(4) . . ?
C7 N1 Mo1 129.2(5) . . ?
C7 N1 N2 114.5(6) . . ?
C13 C9 C8 122.8(7) . . ?
C13 C9 C10 118.7(7) . . ?
C10 C9 C8 118.5(7) . . ?
O5 C5 C6 114.7(7) . . ?
O5 C5 C4 125.3(6) . . ?
C4 C5 C6 120.0(7) . . ?
O1 C2 C1 121.0(6) . . ?
O1 C2 C3 119.5(7) . . ?
C3 C2 C1 119.4(7) . . ?
C5 C6 H6 120.1 . . ?
C5 C6 C1 119.9(7) . . ?
C1 C6 H6 120.1 . . ?
C2 C1 C7 122.7(7) . . ?
C6 C1 C2 119.3(6) . . ?
C6 C1 C7 117.8(7) . . ?
C13 C12 H12 121.2 . . ?
C11 C12 H12 121.2 . . ?
C11 C12 C13 117.5(8) . . ?
O2 C8 C9 116.8(6) . . ?
N2 C8 O2 124.6(6) . . ?
N2 C8 C9 118.5(7) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 C5 119.5(7) . . ?
C3 C4 H4 120.3 . . ?
C2 C3 C4 121.8(7) . . ?
C2 C3 H3A 119.1 . . ?
C4 C3 H3A 119.1 . . ?
C9 C13 C12 120.5(8) . . ?
C9 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
N3 C10 C9 120.1(7) . . ?
N3 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
O5 C14 H14A 109.5 . . ?
O5 C14 H14B 109.5 . . ?
O5 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C11 C12 121.0(8) . . ?
N3 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
N1 C7 C1 122.6(7) . . ?
N1 C7 H7 118.7 . . ?
C1 C7 H7 118.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O2 C8 N2 4.0(10) . . . . ?
Mo1 O2 C8 C9 -178.0(5) . . . . ?
Mo1 O1 C2 C1 -35.4(12) . . . . ?
Mo1 O1 C2 C3 148.9(6) . . . . ?
Mo1 N1 C7 C1 3.5(11) . . . . ?
O9 Mo2 O8 Mo4 -5.0(2) . . . 2_667 ?
O9 Mo3 O12 Mo2 7.9(2) . . . . ?
O9 Mo3 O14 Mo4 1.9(2) . . . 2_667 ?
O9 Mo4 O10 Mo2 -0.8(2) . . . . ?
O8 Mo4 O10 Mo2 6.1(7) 2_667 . . . ?
O12 Mo2 O8 Mo4 -79.9(3) . . . 2_667 ?
O12 Mo3 O14 Mo4 78.6(3) . . . 2_667 ?
O10 Mo2 O8 Mo4 -14.4(7) . . . 2_667 ?
O13 Mo3 O12 Mo2 83.9(3) . . . . ?
O13 Mo3 O14 Mo4 -8.7(7) . . . 2_667 ?
O13 Mo4 O10 Mo2 -77.1(3) . . . . ?
O14 Mo3 O12 Mo2 -68.8(3) . . . . ?
O14 Mo4 O10 Mo2 74.9(3) 2_667 . . . ?
O6 Mo2 O8 Mo4 72.1(3) . . . 2_667 ?
O6 Mo3 O12 Mo2 14.5(7) 2_667 . . . ?
O6 Mo3 O14 Mo4 -75.1(3) 2_667 . . 2_667 ?
O5 C5 C6 C1 178.5(6) . . . . ?
O5 C5 C4 C3 -178.8(7) . . . . ?
O1 C2 C1 C6 -173.5(7) . . . . ?
O1 C2 C1 C7 3.3(12) . . . . ?
O1 C2 C3 C4 173.2(7) . . . . ?
O11 Mo4 O10 Mo2 175.6(3) . . . . ?
O15 Mo3 O12 Mo2 -175.5(3) . . . . ?
O15 Mo3 O14 Mo4 -178.1(3) . . . 2_667 ?
O7 Mo2 O8 Mo4 178.7(3) . . . 2_667 ?
N2 N1 C7 C1 179.3(6) . . . . ?
N1 N2 C8 O2 -1.5(10) . . . . ?
N1 N2 C8 C9 -179.4(6) . . . . ?
C5 C6 C1 C2 0.0(11) . . . . ?
C5 C6 C1 C7 -176.9(7) . . . . ?
C5 C4 C3 C2 0.5(12) . . . . ?
C2 C1 C7 N1 9.1(12) . . . . ?
C6 C5 C4 C3 1.9(12) . . . . ?
C6 C1 C7 N1 -174.1(7) . . . . ?
C1 C2 C3 C4 -2.5(12) . . . . ?
C8 N2 N1 Mo1 -1.4(7) . . . . ?
C8 N2 N1 C7 -177.8(6) . . . . ?
C8 C9 C13 C12 179.2(7) . . . . ?
C8 C9 C10 N3 179.9(7) . . . . ?
C4 C5 C6 C1 -2.1(11) . . . . ?
C3 C2 C1 C6 2.3(11) . . . . ?
C3 C2 C1 C7 179.0(7) . . . . ?
C13 C9 C8 O2 -3.6(11) . . . . ?
C13 C9 C8 N2 174.5(7) . . . . ?
C13 C9 C10 N3 -2.9(12) . . . . ?
C13 C12 C11 N3 0.3(13) . . . . ?
C10 N3 C11 C12 -1.1(13) . . . . ?
C10 C9 C8 O2 173.5(7) . . . . ?
C10 C9 C8 N2 -8.4(11) . . . . ?
C10 C9 C13 C12 2.1(12) . . . . ?
C14 O5 C5 C6 -171.1(7) . . . . ?
C14 O5 C5 C4 9.5(11) . . . . ?
C11 N3 C10 C9 2.4(12) . . . . ?
C11 C12 C13 C9 -0.8(12) . . . . ?

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.035
_oxdiff_exptl_absorpt_empirical_full_min 0.401
# start Validation Reply Form
_vrf_PLAT430_exp_2376            
;
PROBLEM: Short Inter D...A Contact  O4       ..O6       .       2.84 Ang.  
RESPONSE: cis-MoO2 moiety is slightly skewed leading to closer than
expected distances between neighboring oxygen atoms.
However, no indications of errors in modelling the cis-MoO2
moiety were observed.
;
_vrf_PLAT971_exp_2376            
;
PROBLEM: Check Calcd Resid. Dens.  0.84Ang From Mo1             2.60 eA-3  
RESPONSE: Artifact due to insufficient data quality.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1Hw
_database_code_depnum_ccdc_archive 'CCDC 2335837'
loop_
_audit_author_name
_audit_author_address
'Mirta Rubcic'
;University of Zagreb
Croatia
;
_audit_update_record             
;
2024-02-27 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2022-05-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'bis((aquo)-dioxo-(N-(2-oxy-3-methoxybenzylidene)nicotinylhydrazonato)-molybdenum(vi)) hexamolybdate'
_chemical_formula_moiety         '4(C14 H14 Mo N3 O6), 2(Mo6 O19)'
_chemical_formula_sum            'C56 H56 Mo16 N12 O62'
_chemical_formula_weight         3424.16
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.2569(3)
_cell_length_b                   9.2706(2)
_cell_length_c                   21.2974(5)
_cell_angle_alpha                90
_cell_angle_beta                 103.717(2)
_cell_angle_gamma                90
_cell_volume                     2159.17(9)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    6137
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.2690
_cell_measurement_theta_min      4.4450
_shelx_estimated_absorpt_T_max   0.852
_shelx_estimated_absorpt_T_min   0.781
_exptl_absorpt_coefficient_mu    2.359
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.633
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15865
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.927
_diffrn_reflns_theta_min         4.327
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    7.00   90.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4994   19.0000   60.0000 83

#__ type_ start__ end____ width___ exp.time_
  2 omega   17.00   72.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4994   57.0000   90.0000 55

#__ type_ start__ end____ width___ exp.time_
  3 omega   66.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4994  179.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
  4 omega  -33.00   -8.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4994  -57.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
  5 omega   23.00   59.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4994  -99.0000    0.0000 36

#__ type_ start__ end____ width___ exp.time_
  6 omega  -34.00   24.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       22.4994  -57.0000 -120.0000 58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5735
_reflns_number_total             7131
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.155
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         7131
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0347
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0265P)²+2.1483P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0793
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H10(0.024) H7(0.023) H12(0.031) H6(0.027) H14A(0.038) H14B(0.038)
 H14C(0.038) H4(0.027) H5(0.031) H13(0.027)
 Fixed X: O12(0) H10(0.101592) H7(0.463409) H12(0.170148) H6(0.594594)
 H14A(0.593776) H14B(0.631855) H14C(0.722606) H4(0.696157) H5(0.704385)
 H13(0.278077)
 Fixed Y: O12(0) H10(0.741329) H7(0.83823) H12(1.2337) H6(0.77506)
 H14A(0.130365) H14B(0.044834) H14C(0.16217) H4(0.361765) H5(0.606667)
 H13(1.081266)
 Fixed Z: O12(0.5) H10(0.800935) H7(0.624041) H12(0.796641) H6(0.555615)
 H14A(0.544321) H14B(0.611367) H14C(0.59331) H4(0.536868) H5(0.51096)
 H13(0.745377)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.32703(2) 0.49796(3) 0.70581(2) 0.01757(6) Uani 1 1 d . . . . .
Mo4 Mo 0.03896(2) 0.02090(3) 0.39844(2) 0.01821(7) Uani 1 1 d . . . . .
Mo2 Mo 0.20111(2) 0.06418(4) 0.54708(2) 0.02197(7) Uani 1 1 d . . . . .
Mo3 Mo -0.05639(3) 0.24084(3) 0.49597(2) 0.02170(7) Uani 1 1 d . . . . .
O12 O 0.000000 0.000000 0.500000 0.0127(6) Uani 1 2 d S T P . .
O10 O 0.18681(19) 0.0751(3) 0.45052(11) 0.0202(5) Uani 1 1 d . . . . .
O9 O 0.21204(19) -0.1365(3) 0.53487(11) 0.0227(5) Uani 1 1 d . . . . .
O13 O 0.0703(2) -0.1780(3) 0.41805(11) 0.0224(5) Uani 1 1 d . . . . .
O15 O -0.0303(2) 0.2075(3) 0.41164(12) 0.0257(5) Uani 1 1 d . . . . .
O2 O 0.2497(2) 0.6544(3) 0.74825(11) 0.0202(5) Uani 1 1 d . . . . .
O11 O 0.1134(2) 0.2484(3) 0.52989(13) 0.0272(5) Uani 1 1 d . . . . .
O6 O 0.5035(2) 0.5827(3) 0.78460(12) 0.0246(5) Uani 1 1 d D . . . .
O5 O 0.5809(2) 0.2472(2) 0.62053(11) 0.0200(5) Uani 1 1 d . . . . .
O1 O 0.4563(2) 0.4344(2) 0.66766(11) 0.0215(5) Uani 1 1 d . . . . .
O8 O 0.1373(2) 0.0419(3) 0.61866(11) 0.0278(6) Uani 1 1 d . . . . .
O4 O 0.3231(2) 0.3676(3) 0.76203(13) 0.0297(6) Uani 1 1 d . . . . .
O3 O 0.2021(2) 0.4687(3) 0.64530(14) 0.0358(7) Uani 1 1 d . . . . .
O14 O 0.0606(2) 0.0353(3) 0.32254(12) 0.0325(6) Uani 1 1 d . . . . .
N1 N 0.3820(2) 0.7136(3) 0.67252(13) 0.0182(5) Uani 1 1 d . . . . .
O16 O -0.1050(3) 0.4119(3) 0.49520(15) 0.0389(7) Uani 1 1 d . . . . .
O7 O 0.3478(2) 0.1117(4) 0.57588(13) 0.0399(7) Uani 1 1 d . . . . .
N2 N 0.3342(2) 0.8346(3) 0.69748(12) 0.0179(5) Uani 1 1 d . . . . .
N3 N 0.0524(3) 0.9353(4) 0.82838(15) 0.0278(7) Uani 1 1 d D . . . .
C2 C 0.5168(3) 0.4858(3) 0.62513(14) 0.0161(6) Uani 1 1 d . . . . .
C3 C 0.5854(3) 0.3852(4) 0.59856(15) 0.0181(6) Uani 1 1 d . . . . .
C8 C 0.2663(3) 0.7906(3) 0.73536(14) 0.0167(6) Uani 1 1 d . . . . .
C1 C 0.5187(3) 0.6322(4) 0.60803(15) 0.0185(6) Uani 1 1 d . . . . .
C10 C 0.1155(3) 0.8422(4) 0.79932(15) 0.0204(6) Uani 1 1 d . . . . .
H10 H 0.101592 0.741329 0.800935 0.024 Uiso 1 1 calc R . . . .
C7 C 0.4532(3) 0.7403(4) 0.63489(15) 0.0194(6) Uani 1 1 d . . . . .
H7 H 0.463409 0.838230 0.624041 0.023 Uiso 1 1 calc R . . . .
C9 C 0.2007(3) 0.8949(3) 0.76708(14) 0.0172(6) Uani 1 1 d . . . . .
C12 C 0.1558(3) 1.1327(4) 0.79670(17) 0.0255(7) Uani 1 1 d . . . . .
H12 H 0.170148 1.233700 0.796641 0.031 Uiso 1 1 calc R . . . .
C6 C 0.5908(3) 0.6758(4) 0.56609(16) 0.0223(7) Uani 1 1 d . . . . .
H6 H 0.594594 0.775060 0.555615 0.027 Uiso 1 1 calc R . . . .
C14 C 0.6367(3) 0.1375(4) 0.58998(18) 0.0254(7) Uani 1 1 d . . . . .
H14A H 0.593776 0.130365 0.544321 0.038 Uiso 1 1 calc GR . . . .
H14B H 0.631855 0.044834 0.611367 0.038 Uiso 1 1 calc GR . . . .
H14C H 0.722606 0.162170 0.593310 0.038 Uiso 1 1 calc GR . . . .
C4 C 0.6524(3) 0.4305(4) 0.55570(16) 0.0222(7) Uani 1 1 d . . . . .
H4 H 0.696157 0.361765 0.536868 0.027 Uiso 1 1 calc R . . . .
C5 C 0.6566(3) 0.5761(4) 0.53976(17) 0.0255(7) Uani 1 1 d . . . . .
H5 H 0.704385 0.606667 0.510960 0.031 Uiso 1 1 calc R . . . .
C13 C 0.2199(3) 1.0429(4) 0.76670(16) 0.0222(7) Uani 1 1 d . . . . .
H13 H 0.278077 1.081266 0.745377 0.027 Uiso 1 1 calc R . . . .
C11 C 0.0707(4) 1.0794(4) 0.82707(19) 0.0320(9) Uani 1 1 d . . . . .
H11 H 0.039(4) 1.137(5) 0.848(2) 0.044(13) Uiso 1 1 d . . . . .
H6A H 0.550(4) 0.516(4) 0.795(2) 0.047(15) Uiso 1 1 d D . . . .
H6B H 0.505(4) 0.638(4) 0.8140(16) 0.044(14) Uiso 1 1 d D . . . .
H3 H -0.001(4) 0.902(6) 0.847(2) 0.076(19) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O2 2.013(2) . ?
Mo1 O6 2.408(3) . ?
Mo1 O1 1.919(2) . ?
Mo1 O4 1.709(2) . ?
Mo1 O3 1.689(3) . ?
Mo1 N1 2.256(3) . ?
Mo4 O12 2.3147(3) . ?
Mo4 O10 1.838(2) . ?
Mo4 O13 1.905(2) . ?
Mo4 O15 1.945(2) . ?
Mo4 O8 2.017(2) 3_556 ?
Mo4 O14 1.696(2) . ?
Mo2 O12 2.3255(3) . ?
Mo2 O10 2.027(2) . ?
Mo2 O9 1.887(3) . ?
Mo2 O11 1.964(3) . ?
Mo2 O8 1.844(2) . ?
Mo2 O7 1.679(2) . ?
Mo3 O12 2.3172(3) . ?
Mo3 O9 1.972(2) 3_556 ?
Mo3 O13 1.963(2) 3_556 ?
Mo3 O15 1.912(2) . ?
Mo3 O11 1.877(2) . ?
Mo3 O16 1.677(3) . ?
O2 C8 1.315(4) . ?
O5 C3 1.367(4) . ?
O5 C14 1.430(4) . ?
O1 C2 1.343(4) . ?
N1 N2 1.403(4) . ?
N1 C7 1.285(4) . ?
N2 C8 1.301(4) . ?
N3 C10 1.356(4) . ?
N3 C11 1.353(5) . ?
C2 C3 1.411(4) . ?
C2 C1 1.407(4) . ?
C3 C4 1.380(4) . ?
C8 C9 1.474(4) . ?
C1 C7 1.441(4) . ?
C1 C6 1.401(4) . ?
C10 C9 1.394(4) . ?
C9 C13 1.389(5) . ?
C12 C13 1.357(5) . ?
C12 C11 1.369(6) . ?
C6 C5 1.383(5) . ?
C4 C5 1.396(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mo1 O6 79.91(9) . . ?
O2 Mo1 N1 71.49(10) . . ?
O1 Mo1 O2 149.65(10) . . ?
O1 Mo1 O6 79.18(9) . . ?
O1 Mo1 N1 81.19(10) . . ?
O4 Mo1 O2 96.28(11) . . ?
O4 Mo1 O6 84.07(11) . . ?
O4 Mo1 O1 103.16(11) . . ?
O4 Mo1 N1 154.33(12) . . ?
O3 Mo1 O2 95.05(11) . . ?
O3 Mo1 O6 169.79(12) . . ?
O3 Mo1 O1 101.85(12) . . ?
O3 Mo1 O4 105.42(14) . . ?
O3 Mo1 N1 98.23(12) . . ?
N1 Mo1 O6 71.79(9) . . ?
O10 Mo4 O12 78.70(7) . . ?
O10 Mo4 O13 92.20(10) . . ?
O10 Mo4 O15 90.36(10) . . ?
O10 Mo4 O8 154.10(10) . 3_556 ?
O13 Mo4 O12 77.31(7) . . ?
O13 Mo4 O15 152.73(10) . . ?
O13 Mo4 O8 83.31(10) . 3_556 ?
O15 Mo4 O12 76.59(7) . . ?
O15 Mo4 O8 82.62(11) . 3_556 ?
O8 Mo4 O12 75.42(7) 3_556 . ?
O14 Mo4 O12 177.39(9) . . ?
O14 Mo4 O10 103.86(11) . . ?
O14 Mo4 O13 102.95(12) . . ?
O14 Mo4 O15 102.76(12) . . ?
O14 Mo4 O8 102.00(11) . 3_556 ?
O10 Mo2 O12 74.95(6) . . ?
O9 Mo2 O12 77.11(6) . . ?
O9 Mo2 O10 84.35(10) . . ?
O9 Mo2 O11 151.47(10) . . ?
O11 Mo2 O12 75.35(7) . . ?
O11 Mo2 O10 81.48(10) . . ?
O8 Mo2 O12 78.34(7) . . ?
O8 Mo2 O10 153.06(10) . . ?
O8 Mo2 O9 93.11(11) . . ?
O8 Mo2 O11 88.55(11) . . ?
O7 Mo2 O12 176.02(10) . . ?
O7 Mo2 O10 101.07(12) . . ?
O7 Mo2 O9 102.63(13) . . ?
O7 Mo2 O11 104.32(14) . . ?
O7 Mo2 O8 105.64(12) . . ?
O9 Mo3 O12 75.75(7) 3_556 . ?
O13 Mo3 O12 76.18(7) 3_556 . ?
O13 Mo3 O9 84.49(10) 3_556 3_556 ?
O15 Mo3 O12 77.13(7) . . ?
O15 Mo3 O9 86.00(10) . 3_556 ?
O15 Mo3 O13 153.13(10) . 3_556 ?
O11 Mo3 O12 77.11(7) . . ?
O11 Mo3 O9 152.79(10) . 3_556 ?
O11 Mo3 O13 87.20(11) . 3_556 ?
O11 Mo3 O15 89.91(11) . . ?
O16 Mo3 O12 176.17(9) . . ?
O16 Mo3 O9 101.45(12) . 3_556 ?
O16 Mo3 O13 101.07(12) . 3_556 ?
O16 Mo3 O15 105.43(13) . . ?
O16 Mo3 O11 105.57(13) . . ?
Mo4 O12 Mo4 180.0 . 3_556 ?
Mo4 O12 Mo2 90.041(10) . . ?
Mo4 O12 Mo2 89.959(10) 3_556 . ?
Mo4 O12 Mo2 89.958(10) . 3_556 ?
Mo4 O12 Mo2 90.041(10) 3_556 3_556 ?
Mo4 O12 Mo3 89.753(10) . . ?
Mo4 O12 Mo3 89.754(10) 3_556 3_556 ?
Mo4 O12 Mo3 90.247(10) . 3_556 ?
Mo4 O12 Mo3 90.246(10) 3_556 . ?
Mo2 O12 Mo2 180.0 . 3_556 ?
Mo3 O12 Mo2 90.023(11) . 3_556 ?
Mo3 O12 Mo2 90.024(11) 3_556 . ?
Mo3 O12 Mo2 89.977(11) 3_556 3_556 ?
Mo3 O12 Mo2 89.977(11) . . ?
Mo3 O12 Mo3 179.999(15) 3_556 . ?
Mo4 O10 Mo2 116.18(11) . . ?
Mo2 O9 Mo3 116.59(11) . 3_556 ?
Mo4 O13 Mo3 116.12(11) . 3_556 ?
Mo3 O15 Mo4 115.82(12) . . ?
C8 O2 Mo1 120.03(19) . . ?
Mo3 O11 Mo2 117.40(12) . . ?
C3 O5 C14 117.0(3) . . ?
C2 O1 Mo1 137.2(2) . . ?
Mo2 O8 Mo4 116.25(12) . 3_556 ?
N2 N1 Mo1 115.55(19) . . ?
C7 N1 Mo1 128.7(2) . . ?
C7 N1 N2 115.7(3) . . ?
C8 N2 N1 108.6(3) . . ?
C11 N3 C10 121.4(3) . . ?
O1 C2 C3 116.7(3) . . ?
O1 C2 C1 123.9(3) . . ?
C1 C2 C3 119.4(3) . . ?
O5 C3 C2 114.4(3) . . ?
O5 C3 C4 125.5(3) . . ?
C4 C3 C2 120.1(3) . . ?
O2 C8 C9 115.0(3) . . ?
N2 C8 O2 124.3(3) . . ?
N2 C8 C9 120.7(3) . . ?
C2 C1 C7 121.9(3) . . ?
C6 C1 C2 119.3(3) . . ?
C6 C1 C7 118.7(3) . . ?
N3 C10 C9 119.8(3) . . ?
N1 C7 C1 124.5(3) . . ?
C10 C9 C8 118.3(3) . . ?
C13 C9 C8 123.3(3) . . ?
C13 C9 C10 118.4(3) . . ?
C13 C12 C11 120.7(3) . . ?
C5 C6 C1 120.8(3) . . ?
C3 C4 C5 120.6(3) . . ?
C6 C5 C4 119.7(3) . . ?
C12 C13 C9 120.2(3) . . ?
N3 C11 C12 119.5(3) . . ?

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT430_exp_3788            
;
PROBLEM: Short Inter D...A Contact  O16      ..O16      .       2.84 Ang.  
RESPONSE: O16-O16 short contact is a consequence of crystal packing.
All terminal Mo-O distances are in the expected range.
;
_vrf_PLAT910_exp_3788            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         18 Note  
RESPONSE: Low-angle reflections are shadowed by beam-stop, and not
included in integration.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2O-CH3CN-H2O
_database_code_depnum_ccdc_archive 'CCDC 2335835'
loop_
_audit_author_name
_audit_author_address
'Mirta Rubcic'
;University of Zagreb
Croatia
;
_audit_update_record             
;
2024-02-27 deposited with the CCDC.	2024-06-06 downloaded from the CCDC.
;
_audit_creation_date             2024-02-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
"[(?2-oxo)[4-methoxy-2-oxidophenyl)methylidene]pyridin-1-ium-4-carbohydrazone-O,O',N)oxomolybdenum(VI)] {bis-[(?2-oxo)((4-methoxy-2-oxidophenyl)methylidene)pyridin-1-ium-4-carbohydrazidato-O,O',N)oxomolybdenum(VI)] dodecakis(?-oxido)-tetradecaoxooctamolybdenum(VI)}"
_chemical_formula_moiety         
'C28 H25 Mo10 N6 O36, C14 H12 Mo N3 O5, C2 N, C2 H3 N, H2 O'
_chemical_formula_sum            'C46 H42 Mo11 N11 O42'
_chemical_formula_weight         2476.24
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.83910(10)
_cell_length_b                   17.04750(10)
_cell_length_c                   18.70750(10)
_cell_angle_alpha                88.5840(10)
_cell_angle_beta                 84.1140(10)
_cell_angle_gamma                88.5150(10)
_cell_volume                     3436.54(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    62611
_cell_measurement_temperature    170.15
_cell_measurement_theta_max      79.1970
_cell_measurement_theta_min      3.4700
_shelx_estimated_absorpt_T_max   0.373
_shelx_estimated_absorpt_T_min   0.231
_exptl_absorpt_coefficient_mu    16.844
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39513
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.393
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2386
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.073
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            136522
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.395
_diffrn_reflns_theta_min         3.478
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13529
_reflns_number_total             14751
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.92a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.508
_refine_diff_density_min         -1.809
_refine_diff_density_rms         0.168
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1024
_refine_ls_number_reflns         14751
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0389
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0524P)²+16.9348P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1058
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 N10A-C44A
 1.14 with sigma of 0.02
 C44A-N10A
 1.137 with sigma of 0.01
 C44A-C43
 1.456 with sigma of 0.01
 C43-N10A
 2.593 with sigma of 0.02
 C46B-N11B
 1.137 with sigma of 0.01
 N11B-C46B
 1.14 with sigma of 0.02
 C46B-C45B
 1.456 with sigma of 0.01
 C45B-N11B
 2.593 with sigma of 0.02
 N10A-C43
 2.59 with sigma of 0.04
 N11B-C45B
 2.59 with sigma of 0.04
 N10A-C44A \\sim N10B-C44B
 with sigma of 0.02
 N10A-C43 \\sim N10B-C43
 with sigma of 0.04
 C44A-C43 \\sim C44B-C43
 with sigma of 0.02
 N11B-C46B \\sim N11A-C46A
 with sigma of 0.02
 N11B-C45B \\sim N11A-C45A
 with sigma of 0.04
 C46B-C45B \\sim C46A-C45A
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
N10A \\sim C44A \\sim C43: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N11B \\sim C46B \\sim C45B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Uanis(C43) = Uanis(C44B) = Uanis(N10B)
Uanis(C46B) = Uanis(C45B) = Uanis(N11B)
Uanis(C46B) = Uanis(C46A) = Uanis(C45A) = Uanis(N11A)
3. Rigid body (RIGU) restrains
 N10A, C44A, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N11B, C46B, C45B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(O5A)=1-FVAR(1)
 Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(O5B)=FVAR(1)
 Sof(C44B)=Sof(N10B)=1-FVAR(2)
 Sof(N10A)=Sof(C44A)=FVAR(2)
 Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C46A)=Sof(N11A)=1-FVAR(3)
 Sof(N11B)=Sof(C46B)=Sof(C45B)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(3)
5.a Free rotating group:
 O42(H42D,H42E)
5.b Aromatic/amide H refined with riding coordinates:
 N9(H9), N6(H6), N2(H2), N3(H3), C38(H38), C27(H27), C35(H35), C24(H24),
 C26(H26), C34(H34), C39(H39), C21(H21), C13(H13), C33(H33), C11(H11), C10(H10),
  C31(H31), C17(H17), C25(H25), C12(H12), C41(H41), C40(H40), C19(H19), C7(H7),
 C20(H20), C6(H6A), C5(H5), C3(H3A)
5.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C28(H28A,H28B,H28C), C14A(H14A,H14B,H14C), C14B(H14D,
 H14E,H14F), C45B(H45A,H45B,H45C), C45A(H45D,H45E,H45F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo6 Mo 0.36210(3) 0.49505(2) 0.33295(2) 0.01557(8) Uani 1 1 d . . . . .
Mo9 Mo 0.31422(3) 0.65684(2) 0.21151(2) 0.01617(8) Uani 1 1 d . . . . .
Mo3 Mo 0.39666(3) 0.39527(2) 0.17437(2) 0.01715(8) Uani 1 1 d . . . . .
Mo5 Mo 0.14863(3) 0.50730(2) 0.20086(2) 0.01698(8) Uani 1 1 d . . . . .
Mo7 Mo 0.52996(3) 0.64723(2) 0.33892(2) 0.01770(8) Uani 1 1 d . . . . .
Mo4 Mo 0.56458(3) 0.55025(2) 0.18229(2) 0.01837(8) Uani 1 1 d . . . . .
Mo2 Mo 0.61349(3) 0.21861(2) 0.14669(2) 0.01749(8) Uani 1 1 d . . . . .
Mo8 Mo 0.11368(3) 0.59986(2) 0.36476(2) 0.01813(8) Uani 1 1 d . . . . .
Mo10 Mo 0.28075(4) 0.75700(2) 0.37252(2) 0.01918(9) Uani 1 1 d . . . . .
Mo11 Mo 0.04303(4) 0.93335(2) 0.40023(2) 0.02046(9) Uani 1 1 d . . . . .
Mo1 Mo 0.95452(4) 0.11079(3) 0.11705(2) 0.03202(11) Uani 1 1 d . . . . .
O21 O 0.5258(3) 0.53673(18) 0.30498(17) 0.0181(6) Uani 1 1 d . . . . .
O28 O 0.1822(3) 0.49732(17) 0.32423(17) 0.0174(6) Uani 1 1 d . . . . .
O25 O 0.4928(3) 0.65216(18) 0.21992(17) 0.0191(6) Uani 1 1 d . . . . .
O15 O 0.2223(3) 0.40300(18) 0.20107(17) 0.0196(6) Uani 1 1 d . . . . .
O20 O 0.3523(3) 0.53103(17) 0.20918(16) 0.0163(6) Uani 1 1 d . . . . .
O8 O 0.6719(3) 0.29284(18) 0.21640(17) 0.0203(6) Uani 1 1 d . . . . .
O14 O 0.5536(3) 0.43965(19) 0.18521(18) 0.0215(7) Uani 1 1 d . . . . .
O29 O 0.1498(3) 0.61479(18) 0.23752(17) 0.0187(6) Uani 1 1 d . . . . .
O38 O -0.0085(3) 0.85443(19) 0.33138(17) 0.0225(7) Uani 1 1 d . . . . .
O13 O 0.3901(3) 0.40286(18) 0.29425(17) 0.0183(6) Uani 1 1 d . . . . .
O26 O 0.4543(3) 0.74808(19) 0.34000(18) 0.0211(7) Uani 1 1 d . . . . .
O30 O 0.2827(3) 0.74787(18) 0.25058(17) 0.0209(7) Uani 1 1 d . . . . .
O27 O 0.3216(3) 0.61782(17) 0.33313(16) 0.0162(6) Uani 1 1 d . . . . .
O11 O 0.4314(3) 0.29572(19) 0.17988(18) 0.0219(7) Uani 1 1 d . . . . .
O18 O 0.1530(3) 0.5288(2) 0.11146(19) 0.0254(7) Uani 1 1 d . . . . .
O33 O 0.1249(3) 0.71047(19) 0.36434(19) 0.0231(7) Uani 1 1 d . . . . .
O16 O 0.7169(3) 0.5629(2) 0.1923(2) 0.0266(7) Uani 1 1 d . . . . .
O23 O 0.5217(3) 0.6234(2) 0.42858(19) 0.0240(7) Uani 1 1 d . . . . .
O22 O 0.3658(3) 0.4789(2) 0.42227(18) 0.0240(7) Uani 1 1 d . . . . .
O34 O 0.2917(4) 0.7363(2) 0.46121(19) 0.0280(8) Uani 1 1 d . . . . .
O7 O 0.4942(3) 0.1434(2) 0.12598(18) 0.0262(7) Uani 1 1 d . . . . .
O9 O 0.6210(4) 0.2818(2) 0.07444(19) 0.0298(8) Uani 1 1 d . . . . .
O12 O 0.3962(3) 0.4169(2) 0.08460(19) 0.0253(7) Uani 1 1 d . . . . .
O35 O 0.1234(4) 0.5762(2) 0.4529(2) 0.0303(8) Uani 1 1 d . . . . .
O31 O 0.3121(3) 0.6726(2) 0.12188(18) 0.0239(7) Uani 1 1 d . . . . .
O19 O -0.0015(3) 0.4835(2) 0.22741(18) 0.0238(7) Uani 1 1 d . . . . .
O17 O 0.5510(4) 0.5681(2) 0.09275(19) 0.0273(8) Uani 1 1 d . . . . .
O37 O 0.1621(4) 1.0077(2) 0.42336(18) 0.0276(8) Uani 1 1 d . . . . .
O2 O 0.9721(4) 0.1935(2) 0.19082(19) 0.0320(8) Uani 1 1 d . . . . .
O32 O -0.0388(3) 0.5913(2) 0.3528(2) 0.0273(8) Uani 1 1 d . . . . .
O24 O 0.6827(3) 0.6666(2) 0.31506(19) 0.0249(7) Uani 1 1 d . . . . .
O40 O 0.0407(4) 0.8698(2) 0.47195(19) 0.0288(8) Uani 1 1 d . . . . .
O36 O 0.2443(3) 0.85517(19) 0.36784(18) 0.0243(7) Uani 1 1 d . . . . .
O6 O 0.7448(3) 0.1608(2) 0.13519(18) 0.0254(7) Uani 1 1 d . . . . .
N7 N 0.1153(4) 0.9709(2) 0.28998(19) 0.0178(7) Uani 1 1 d . . . . .
O41 O 0.2894(4) 1.2686(2) 0.4537(2) 0.0368(9) Uani 1 1 d . . . . .
N4 N 0.5602(4) 0.1726(2) 0.2574(2) 0.0182(7) Uani 1 1 d . . . . .
N9 N -0.1046(4) 0.6806(2) 0.2053(2) 0.0270(9) Uani 1 1 d . . . . .
H9 H -0.155097 0.644452 0.224595 0.032 Uiso 1 1 calc R U . . .
N8 N 0.0975(4) 0.9192(2) 0.2348(2) 0.0199(8) Uani 1 1 d . . . . .
O1 O 0.8695(5) 0.0234(2) 0.0852(2) 0.0430(10) Uani 1 1 d . . . . .
N5 N 0.5821(4) 0.2212(2) 0.3134(2) 0.0211(8) Uani 1 1 d . . . . .
N6 N 0.6384(5) 0.4090(3) 0.4445(2) 0.0305(10) Uani 1 1 d . . . . .
H6 H 0.603520 0.410416 0.489074 0.037 Uiso 1 1 calc R U . . .
O4 O 0.9577(4) 0.1733(3) 0.0452(2) 0.0433(10) Uani 1 1 d . . . . .
O39 O -0.0894(4) 0.9874(2) 0.4106(2) 0.0345(9) Uani 1 1 d . . . . .
O10 O 0.3456(5) -0.1155(3) 0.0979(3) 0.0484(11) Uani 1 1 d . . . . .
N2 N 0.8784(4) 0.1155(3) 0.2815(2) 0.0269(9) Uani 1 1 d . . . . .
H2 H 0.850104 0.105184 0.326450 0.032 Uiso 1 1 calc R U . . .
N3 N 1.0455(5) 0.3566(3) 0.3408(2) 0.0321(10) Uani 1 1 d . . . . .
H3 H 1.084763 0.399460 0.326037 0.039 Uiso 1 1 calc R U . . .
C36 C 0.0331(4) 0.8612(3) 0.2630(2) 0.0192(9) Uani 1 1 d . . . . .
O42 O 0.6499(5) 0.4328(3) 0.0007(3) 0.0480(11) Uani 1 1 d G . . . .
H42D H 0.658076 0.460979 -0.038869 0.072 Uiso 1 1 d G U . . .
H42E H 0.623079 0.466042 0.033681 0.072 Uiso 1 1 d G U . . .
C38 C -0.0747(4) 0.7381(3) 0.2465(3) 0.0239(10) Uani 1 1 d . . . . .
H38 H -0.105068 0.738556 0.296022 0.029 Uiso 1 1 calc R U . . .
N1 N 0.8687(4) 0.0664(3) 0.2238(2) 0.0284(9) Uani 1 1 d . . . . .
C29 C 0.2037(4) 1.0924(3) 0.3194(3) 0.0204(9) Uani 1 1 d . . . . .
C22 C 0.6378(4) 0.2830(3) 0.2860(2) 0.0193(9) Uani 1 1 d . . . . .
C27 C 0.7443(5) 0.4066(3) 0.3057(3) 0.0242(10) Uani 1 1 d . . . . .
H27 H 0.780182 0.406154 0.257246 0.029 Uiso 1 1 calc R U . . .
C23 C 0.6664(4) 0.3468(3) 0.3326(2) 0.0195(9) Uani 1 1 d . . . . .
C35 C 0.1729(4) 1.0343(3) 0.2704(2) 0.0186(9) Uani 1 1 d . . . . .
H35 H 0.196351 1.043033 0.220534 0.022 Uiso 1 1 calc R U . . .
C8 C 0.9355(5) 0.1785(3) 0.2588(3) 0.0252(10) Uani 1 1 d . . . . .
C37 C 0.0009(4) 0.7976(3) 0.2171(2) 0.0206(9) Uani 1 1 d . . . . .
C24 C 0.6132(5) 0.3497(3) 0.4037(3) 0.0253(10) Uani 1 1 d . . . . .
H24 H 0.559236 0.309669 0.422895 0.030 Uiso 1 1 calc R U . . .
O3 O 1.0996(5) 0.0718(3) 0.1153(2) 0.0550(14) Uani 1 1 d . . . . .
C26 C 0.7690(5) 0.4665(3) 0.3502(3) 0.0271(11) Uani 1 1 d . . . . .
H26 H 0.822926 0.507246 0.332648 0.033 Uiso 1 1 calc R U . . .
C32 C 0.2639(5) 1.2076(3) 0.4130(3) 0.0261(10) Uani 1 1 d . . . . .
C34 C 0.2482(4) 1.1652(3) 0.2931(3) 0.0222(9) Uani 1 1 d . . . . .
H34 H 0.258365 1.175196 0.242635 0.027 Uiso 1 1 calc R U . . .
C39 C -0.0619(5) 0.6750(3) 0.1364(3) 0.0311(11) Uani 1 1 d . . . . .
H39 H -0.084213 0.632123 0.109324 0.037 Uiso 1 1 calc R U . . .
C21 C 0.5170(4) 0.1047(3) 0.2757(3) 0.0220(9) Uani 1 1 d . . . . .
H21 H 0.507765 0.090218 0.325259 0.026 Uiso 1 1 calc R U . . .
C13 C 0.9283(5) 0.2238(3) 0.3860(3) 0.0289(11) Uani 1 1 d . . . . .
H13 H 0.888774 0.176680 0.402639 0.035 Uiso 1 1 calc R U . . .
C33 C 0.2777(5) 1.2227(3) 0.3387(3) 0.0256(10) Uani 1 1 d . . . . .
H33 H 0.306889 1.271878 0.319965 0.031 Uiso 1 1 calc R U . . .
C11 C 1.0149(5) 0.3459(3) 0.4109(3) 0.0324(12) Uani 1 1 d . . . . .
H11 H 1.034280 0.384069 0.443942 0.039 Uiso 1 1 calc R U . . .
C30 C 0.1955(4) 1.0777(3) 0.3937(3) 0.0210(9) Uani 1 1 d . . . . .
C10 C 1.0196(5) 0.3051(3) 0.2911(3) 0.0306(11) Uani 1 1 d . . . . .
H10 H 1.043089 0.315915 0.241608 0.037 Uiso 1 1 calc R U . . .
C15 C 0.4820(5) 0.0497(3) 0.2254(3) 0.0232(10) Uani 1 1 d . . . . .
C31 C 0.2266(5) 1.1346(3) 0.4408(3) 0.0269(10) Uani 1 1 d . . . . .
H31 H 0.222287 1.123577 0.491008 0.032 Uiso 1 1 calc R U . . .
C9 C 0.9592(5) 0.2369(3) 0.3122(3) 0.0260(10) Uani 1 1 d . . . . .
C17 C 0.4214(5) 0.0173(3) 0.1084(3) 0.0323(12) Uani 1 1 d . . . . .
H17 H 0.409180 0.031975 0.060306 0.039 Uiso 1 1 calc R U . . .
C25 C 0.7149(6) 0.4669(3) 0.4204(3) 0.0329(12) Uani 1 1 d . . . . .
H25 H 0.731673 0.507695 0.451450 0.040 Uiso 1 1 calc R U . . .
C12 C 0.9549(6) 0.2788(4) 0.4348(3) 0.0370(13) Uani 1 1 d . . . . .
H12 H 0.931706 0.270293 0.484654 0.044 Uiso 1 1 calc R U . . .
C16 C 0.4683(4) 0.0701(3) 0.1532(3) 0.0232(10) Uani 1 1 d . . . . .
C41 C 0.0458(5) 0.7938(3) 0.1449(3) 0.0296(11) Uani 1 1 d . . . . .
H41 H 0.097594 0.833753 0.123189 0.035 Uiso 1 1 calc R U . . .
C40 C 0.0143(6) 0.7314(3) 0.1047(3) 0.0356(13) Uani 1 1 d . . . . .
H40 H 0.045434 0.727808 0.055547 0.043 Uiso 1 1 calc R U . . .
C18 C 0.3920(5) -0.0587(3) 0.1355(4) 0.0356(13) Uani 1 1 d . . . . .
C19 C 0.4069(6) -0.0798(3) 0.2062(4) 0.0362(13) Uani 1 1 d . . . . .
H19 H 0.387288 -0.131199 0.223814 0.043 Uiso 1 1 calc R U . . .
C7 C 0.8083(5) 0.0027(3) 0.2395(3) 0.0309(11) Uani 1 1 d . . . . .
H7 H 0.780128 -0.008079 0.288402 0.037 Uiso 1 1 calc R U . . .
C20 C 0.4498(5) -0.0264(3) 0.2503(3) 0.0300(11) Uani 1 1 d . . . . .
H20 H 0.458143 -0.040913 0.298994 0.036 Uiso 1 1 calc R U . . .
C1 C 0.7820(5) -0.0516(3) 0.1875(3) 0.0338(12) Uani 1 1 d . . . . .
C2 C 0.8113(6) -0.0412(4) 0.1136(3) 0.0372(13) Uani 1 1 d . . . . .
C6 C 0.7167(5) -0.1205(4) 0.2104(4) 0.0408(14) Uani 1 1 d . . . . .
H6A H 0.695834 -0.130057 0.260396 0.049 Uiso 1 1 calc R U . . .
C42 C 0.2603(7) 1.2596(4) 0.5301(3) 0.0451(16) Uani 1 1 d . . . . .
H42A H 0.174411 1.242883 0.540541 0.068 Uiso 1 1 calc R U . . .
H42B H 0.270316 1.309836 0.552931 0.068 Uiso 1 1 calc R U . . .
H42C H 0.316427 1.219967 0.548837 0.068 Uiso 1 1 calc R U . . .
C5 C 0.6830(6) -0.1737(5) 0.1621(5) 0.0552(19) Uani 1 1 d . . . . .
H5 H 0.638361 -0.219009 0.178649 0.066 Uiso 1 1 calc R U . . .
C3 C 0.7797(6) -0.0948(5) 0.0646(4) 0.0515(18) Uani 1 1 d . . . . .
H3A H 0.802156 -0.086600 0.014641 0.062 Uiso 1 1 calc R U . . .
C28 C 0.3072(9) -0.0945(5) 0.0309(4) 0.060(2) Uani 1 1 d . . . . .
H28A H 0.376916 -0.072304 0.000144 0.089 Uiso 1 1 calc R U . . .
H28B H 0.239346 -0.055384 0.037113 0.089 Uiso 1 1 calc R U . . .
H28C H 0.278427 -0.141098 0.008506 0.089 Uiso 1 1 calc R U . . .
C4 C 0.7144(7) -0.1609(5) 0.0896(5) 0.062(2) Uani 1 1 d . . . . .
C14A C 0.698(3) -0.2292(14) -0.0154(13) 0.061(8) Uani 0.334(17) 1 d . . P A 1
H14A H 0.661755 -0.274206 -0.036570 0.091 Uiso 0.334(17) 1 calc R U P A 1
H14B H 0.786620 -0.227417 -0.031703 0.091 Uiso 0.334(17) 1 calc R U P A 1
H14C H 0.656460 -0.180693 -0.030382 0.091 Uiso 0.334(17) 1 calc R U P A 1
O5B O 0.6808(14) -0.2375(8) 0.0646(8) 0.039(5) Uani 0.334(17) 1 d . . P A 1
C14B C 0.6017(14) -0.2613(8) 0.0500(7) 0.069(4) Uani 0.666(17) 1 d . . P A 2
H14D H 0.579464 -0.286397 0.006707 0.104 Uiso 0.666(17) 1 calc R U P A 2
H14E H 0.526470 -0.240862 0.077561 0.104 Uiso 0.666(17) 1 calc R U P A 2
H14F H 0.643347 -0.299898 0.079586 0.104 Uiso 0.666(17) 1 calc R U P A 2
O5A O 0.6829(8) -0.1985(6) 0.0300(5) 0.053(3) Uani 0.666(17) 1 d . . P A 2
N10A N 0.6043(9) -0.0384(5) 0.4110(5) 0.061(3) Uani 0.694(9) 1 d D U P B 1
C44A C 0.6278(10) 0.0185(5) 0.4372(5) 0.046(2) Uani 0.694(9) 1 d D U P B 1
C43 C 0.6521(8) 0.0927(4) 0.4714(4) 0.0558(17) Uani 1 1 d D U . . .
C44B C 0.5501(19) 0.0857(15) 0.5305(11) 0.0558(17) Uani 0.306(9) 1 d D . P B 2
N10B N 0.4692(18) 0.0744(13) 0.5749(10) 0.0558(17) Uani 0.306(9) 1 d D . P B 2
N11B N 1.1145(13) -0.3908(12) -0.0697(9) 0.102(3) Uani 0.597(10) 1 d D U P C 1
C46B C 1.0115(14) -0.3731(14) -0.0617(11) 0.102(3) Uani 0.597(10) 1 d D U P C 1
C45B C 0.8902(14) -0.3348(12) -0.0598(10) 0.102(3) Uani 0.597(10) 1 d D U P C 1
H45A H 0.871518 -0.321952 -0.108961 0.153 Uiso 0.597(10) 1 calc R U P C 1
H45B H 0.889838 -0.286430 -0.032470 0.153 Uiso 0.597(10) 1 calc R U P C 1
H45C H 0.827248 -0.369966 -0.036684 0.153 Uiso 0.597(10) 1 calc R U P C 1
C45A C 1.043(3) -0.3692(19) -0.0928(16) 0.102(3) Uani 0.403(10) 1 d D . P C 2
H45D H 1.039665 -0.363672 -0.144917 0.153 Uiso 0.403(10) 1 calc R U P C 2
H45E H 1.088560 -0.325711 -0.075999 0.153 Uiso 0.403(10) 1 calc R U P C 2
H45F H 0.957875 -0.368302 -0.068758 0.153 Uiso 0.403(10) 1 calc R U P C 2
C46A C 1.105(3) -0.4437(19) -0.0762(16) 0.102(3) Uani 0.403(10) 1 d D . P C 2
N11A N 1.130(2) -0.5031(16) -0.0562(12) 0.102(3) Uani 0.403(10) 1 d D . P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo6 Mo7 3.2178(5) . ?
Mo6 Mo8 3.2050(5) . ?
Mo6 O21 1.945(3) . ?
Mo6 O28 1.973(3) . ?
Mo6 O20 2.393(3) . ?
Mo6 O13 1.753(3) . ?
Mo6 O27 2.127(3) . ?
Mo6 O22 1.691(3) . ?
Mo9 Mo5 3.1774(5) . ?
Mo9 O25 1.957(3) . ?
Mo9 O20 2.174(3) . ?
Mo9 O29 1.949(3) . ?
Mo9 O30 1.743(3) . ?
Mo9 O27 2.363(3) . ?
Mo9 O31 1.694(3) . ?
Mo3 O15 1.907(3) . ?
Mo3 O20 2.442(3) . ?
Mo3 O14 1.911(3) . ?
Mo3 O13 2.243(3) . ?
Mo3 O11 1.732(3) . ?
Mo3 O12 1.711(3) . ?
Mo5 O28 2.374(3) . ?
Mo5 O15 1.930(3) . ?
Mo5 O20 2.276(3) . ?
Mo5 O29 1.973(3) . ?
Mo5 O18 1.699(3) . ?
Mo5 O19 1.708(3) . ?
Mo7 O21 2.006(3) . ?
Mo7 O25 2.302(3) . ?
Mo7 O26 1.885(3) . ?
Mo7 O27 2.340(3) . ?
Mo7 O23 1.710(3) . ?
Mo7 O24 1.708(3) . ?
Mo4 O21 2.298(3) . ?
Mo4 O25 1.999(3) . ?
Mo4 O20 2.334(3) . ?
Mo4 O14 1.891(3) . ?
Mo4 O16 1.700(4) . ?
Mo4 O17 1.716(4) . ?
Mo2 O8 1.999(3) . ?
Mo2 O11 2.380(3) . ?
Mo2 O7 1.919(3) . ?
Mo2 O9 1.704(4) . ?
Mo2 O6 1.709(3) . ?
Mo2 N4 2.222(4) . ?
Mo8 O28 2.016(3) . ?
Mo8 O29 2.381(3) . ?
Mo8 O27 2.297(3) . ?
Mo8 O33 1.892(3) . ?
Mo8 O35 1.702(4) . ?
Mo8 O32 1.701(4) . ?
Mo10 O26 1.920(3) . ?
Mo10 O30 2.288(3) . ?
Mo10 O27 2.517(3) . ?
Mo10 O33 1.907(3) . ?
Mo10 O34 1.703(4) . ?
Mo10 O36 1.712(3) . ?
Mo11 O38 2.013(3) . ?
Mo11 O37 1.920(4) . ?
Mo11 O40 1.702(3) . ?
Mo11 N7 2.215(4) . ?
Mo11 O39 1.682(4) . ?
Mo1 O2 2.023(4) . ?
Mo1 O6 2.401(3) . ?
Mo1 O1 1.911(5) . ?
Mo1 O4 1.693(4) . ?
Mo1 N1 2.237(4) . ?
Mo1 O3 1.688(4) . ?
O8 C22 1.325(5) . ?
O38 C36 1.315(6) . ?
O7 C16 1.362(6) . ?
O37 C30 1.346(6) . ?
O2 C8 1.313(6) . ?
N7 N8 1.405(5) . ?
N7 C35 1.288(6) . ?
O41 C32 1.354(6) . ?
O41 C42 1.436(7) . ?
N4 N5 1.394(5) . ?
N4 C21 1.286(6) . ?
N9 H9 0.8800 . ?
N9 C38 1.329(6) . ?
N9 C39 1.329(7) . ?
N8 C36 1.296(6) . ?
O1 C2 1.353(8) . ?
N5 C22 1.296(6) . ?
N6 H6 0.8800 . ?
N6 C24 1.332(7) . ?
N6 C25 1.344(8) . ?
O10 C18 1.348(7) . ?
O10 C28 1.396(9) . ?
N2 H2 0.8800 . ?
N2 N1 1.397(6) . ?
N2 C8 1.294(7) . ?
N3 H3 0.8800 . ?
N3 C11 1.328(7) . ?
N3 C10 1.348(7) . ?
C36 C37 1.470(6) . ?
O42 H42D 0.8705 . ?
O42 H42E 0.8711 . ?
C38 H38 0.9500 . ?
C38 C37 1.387(7) . ?
N1 C7 1.294(7) . ?
C29 C35 1.435(6) . ?
C29 C34 1.404(6) . ?
C29 C30 1.400(7) . ?
C22 C23 1.469(6) . ?
C27 H27 0.9500 . ?
C27 C23 1.391(7) . ?
C27 C26 1.382(7) . ?
C23 C24 1.396(7) . ?
C35 H35 0.9500 . ?
C8 C9 1.473(7) . ?
C37 C41 1.391(7) . ?
C24 H24 0.9500 . ?
C26 H26 0.9500 . ?
C26 C25 1.383(8) . ?
C32 C33 1.401(7) . ?
C32 C31 1.391(7) . ?
C34 H34 0.9500 . ?
C34 C33 1.380(7) . ?
C39 H39 0.9500 . ?
C39 C40 1.367(8) . ?
C21 H21 0.9500 . ?
C21 C15 1.428(7) . ?
C13 H13 0.9500 . ?
C13 C9 1.402(7) . ?
C13 C12 1.380(8) . ?
C33 H33 0.9500 . ?
C11 H11 0.9500 . ?
C11 C12 1.373(8) . ?
C30 C31 1.396(7) . ?
C10 H10 0.9500 . ?
C10 C9 1.379(7) . ?
C15 C16 1.408(7) . ?
C15 C20 1.407(7) . ?
C31 H31 0.9500 . ?
C17 H17 0.9500 . ?
C17 C16 1.386(7) . ?
C17 C18 1.411(8) . ?
C25 H25 0.9500 . ?
C12 H12 0.9500 . ?
C41 H41 0.9500 . ?
C41 C40 1.388(7) . ?
C40 H40 0.9500 . ?
C18 C19 1.386(9) . ?
C19 H19 0.9500 . ?
C19 C20 1.367(8) . ?
C7 H7 0.9500 . ?
C7 C1 1.414(8) . ?
C20 H20 0.9500 . ?
C1 C2 1.394(9) . ?
C1 C6 1.421(9) . ?
C2 C3 1.384(9) . ?
C6 H6A 0.9500 . ?
C6 C5 1.380(9) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C5 H5 0.9500 . ?
C5 C4 1.377(12) . ?
C3 H3A 0.9500 . ?
C3 C4 1.390(12) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C4 O5B 1.466(15) . ?
C4 O5A 1.378(11) . ?
C14A H14A 0.9800 . ?
C14A H14B 0.9800 . ?
C14A H14C 0.9800 . ?
C14A O5B 1.49(3) . ?
C14B H14D 0.9800 . ?
C14B H14E 0.9800 . ?
C14B H14F 0.9800 . ?
C14B O5A 1.422(14) . ?
N10A C44A 1.144(7) . ?
C44A C43 1.472(7) . ?
C43 C44B 1.487(16) . ?
C44B N10B 1.161(17) . ?
N11B C46B 1.144(8) . ?
C46B C45B 1.451(9) . ?
C45B H45A 0.9800 . ?
C45B H45B 0.9800 . ?
C45B H45C 0.9800 . ?
C45A H45D 0.9800 . ?
C45A H45E 0.9800 . ?
C45A H45F 0.9800 . ?
C45A C46A 1.46(2) . ?
C46A N11A 1.110(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Mo8 Mo6 Mo7 90.948(12) . . ?
O21 Mo6 Mo7 36.10(9) . . ?
O21 Mo6 Mo8 124.68(9) . . ?
O21 Mo6 O28 149.61(13) . . ?
O21 Mo6 O20 77.34(12) . . ?
O21 Mo6 O27 78.98(12) . . ?
O28 Mo6 Mo7 125.19(9) . . ?
O28 Mo6 Mo8 37.00(9) . . ?
O28 Mo6 O20 77.30(12) . . ?
O28 Mo6 O27 78.60(12) . . ?
O20 Mo6 Mo7 85.67(7) . . ?
O20 Mo6 Mo8 86.29(7) . . ?
O13 Mo6 Mo7 132.93(10) . . ?
O13 Mo6 Mo8 132.14(11) . . ?
O13 Mo6 O21 96.84(14) . . ?
O13 Mo6 O28 95.14(14) . . ?
O13 Mo6 O20 80.34(12) . . ?
O13 Mo6 O27 155.59(13) . . ?
O27 Mo6 Mo7 46.62(8) . . ?
O27 Mo6 Mo8 45.70(8) . . ?
O27 Mo6 O20 75.27(11) . . ?
O22 Mo6 Mo7 90.49(12) . . ?
O22 Mo6 Mo8 89.72(12) . . ?
O22 Mo6 O21 101.85(15) . . ?
O22 Mo6 O28 101.75(15) . . ?
O22 Mo6 O20 174.41(14) . . ?
O22 Mo6 O13 105.24(16) . . ?
O22 Mo6 O27 99.14(14) . . ?
O25 Mo9 Mo5 124.29(9) . . ?
O25 Mo9 O20 78.56(12) . . ?
O25 Mo9 O27 77.80(12) . . ?
O20 Mo9 Mo5 45.74(8) . . ?
O20 Mo9 O27 75.06(11) . . ?
O29 Mo9 Mo5 36.15(9) . . ?
O29 Mo9 O25 149.42(13) . . ?
O29 Mo9 O20 78.07(12) . . ?
O29 Mo9 O27 77.32(12) . . ?
O30 Mo9 Mo5 132.19(11) . . ?
O30 Mo9 O25 97.55(15) . . ?
O30 Mo9 O20 156.47(13) . . ?
O30 Mo9 O29 96.05(15) . . ?
O30 Mo9 O27 81.43(13) . . ?
O27 Mo9 Mo5 85.69(7) . . ?
O31 Mo9 Mo5 89.02(11) . . ?
O31 Mo9 O25 101.23(15) . . ?
O31 Mo9 O20 97.68(14) . . ?
O31 Mo9 O29 101.20(15) . . ?
O31 Mo9 O30 105.83(16) . . ?
O31 Mo9 O27 172.73(14) . . ?
O15 Mo3 O20 73.74(12) . . ?
O15 Mo3 O14 145.07(14) . . ?
O15 Mo3 O13 78.74(13) . . ?
O14 Mo3 O20 74.02(12) . . ?
O14 Mo3 O13 78.31(13) . . ?
O13 Mo3 O20 70.78(11) . . ?
O11 Mo3 O15 104.40(15) . . ?
O11 Mo3 O20 161.03(13) . . ?
O11 Mo3 O14 101.69(15) . . ?
O11 Mo3 O13 90.28(13) . . ?
O12 Mo3 O15 98.37(15) . . ?
O12 Mo3 O20 93.43(14) . . ?
O12 Mo3 O14 96.60(16) . . ?
O12 Mo3 O13 164.17(14) . . ?
O12 Mo3 O11 105.48(16) . . ?
O28 Mo5 Mo9 80.29(7) . . ?
O15 Mo5 Mo9 120.58(10) . . ?
O15 Mo5 O28 81.60(12) . . ?
O15 Mo5 O20 77.41(12) . . ?
O15 Mo5 O29 146.66(13) . . ?
O20 Mo5 Mo9 43.17(7) . . ?
O20 Mo5 O28 72.35(11) . . ?
O29 Mo5 Mo9 35.63(9) . . ?
O29 Mo5 O28 72.32(12) . . ?
O29 Mo5 O20 75.16(12) . . ?
O18 Mo5 Mo9 86.86(12) . . ?
O18 Mo5 O28 166.59(14) . . ?
O18 Mo5 O15 101.93(15) . . ?
O18 Mo5 O20 95.61(14) . . ?
O18 Mo5 O29 99.28(15) . . ?
O18 Mo5 O19 105.38(17) . . ?
O19 Mo5 Mo9 135.84(11) . . ?
O19 Mo5 O28 86.68(14) . . ?
O19 Mo5 O15 98.59(15) . . ?
O19 Mo5 O20 158.99(14) . . ?
O19 Mo5 O29 100.22(15) . . ?
O21 Mo7 Mo6 34.85(9) . . ?
O21 Mo7 O25 71.93(12) . . ?
O21 Mo7 O27 72.83(12) . . ?
O25 Mo7 Mo6 79.50(8) . . ?
O25 Mo7 O27 72.08(11) . . ?
O26 Mo7 Mo6 119.59(10) . . ?
O26 Mo7 O21 146.44(14) . . ?
O26 Mo7 O25 83.35(13) . . ?
O26 Mo7 O27 78.24(13) . . ?
O27 Mo7 Mo6 41.36(7) . . ?
O23 Mo7 Mo6 83.35(11) . . ?
O23 Mo7 O21 96.08(15) . . ?
O23 Mo7 O25 162.35(14) . . ?
O23 Mo7 O26 101.78(15) . . ?
O23 Mo7 O27 92.26(14) . . ?
O24 Mo7 Mo6 134.51(12) . . ?
O24 Mo7 O21 99.81(15) . . ?
O24 Mo7 O25 90.35(14) . . ?
O24 Mo7 O26 102.75(16) . . ?
O24 Mo7 O27 162.26(14) . . ?
O24 Mo7 O23 104.72(17) . . ?
O21 Mo4 O20 72.31(11) . . ?
O25 Mo4 O21 72.14(12) . . ?
O25 Mo4 O20 73.97(12) . . ?
O14 Mo4 O21 83.47(13) . . ?
O14 Mo4 O25 146.54(14) . . ?
O14 Mo4 O20 77.04(13) . . ?
O16 Mo4 O21 89.06(15) . . ?
O16 Mo4 O25 100.03(15) . . ?
O16 Mo4 O20 161.35(15) . . ?
O16 Mo4 O14 102.15(16) . . ?
O16 Mo4 O17 105.35(18) . . ?
O17 Mo4 O21 164.10(15) . . ?
O17 Mo4 O25 98.23(15) . . ?
O17 Mo4 O20 93.07(15) . . ?
O17 Mo4 O14 99.66(15) . . ?
O8 Mo2 O11 77.63(13) . . ?
O8 Mo2 N4 71.51(13) . . ?
O7 Mo2 O8 148.29(14) . . ?
O7 Mo2 O11 82.31(14) . . ?
O7 Mo2 N4 80.76(14) . . ?
O9 Mo2 O8 96.96(16) . . ?
O9 Mo2 O11 81.29(15) . . ?
O9 Mo2 O7 104.04(17) . . ?
O9 Mo2 O6 105.71(17) . . ?
O9 Mo2 N4 158.84(16) . . ?
O6 Mo2 O8 97.71(15) . . ?
O6 Mo2 O11 172.14(14) . . ?
O6 Mo2 O7 99.11(16) . . ?
O6 Mo2 N4 93.62(15) . . ?
N4 Mo2 O11 78.94(13) . . ?
O28 Mo8 Mo6 36.07(9) . . ?
O28 Mo8 O29 71.49(12) . . ?
O28 Mo8 O27 73.82(12) . . ?
O29 Mo8 Mo6 79.15(8) . . ?
O27 Mo8 Mo6 41.53(7) . . ?
O27 Mo8 O29 70.88(11) . . ?
O33 Mo8 Mo6 119.09(11) . . ?
O33 Mo8 O28 147.40(14) . . ?
O33 Mo8 O29 84.59(13) . . ?
O33 Mo8 O27 77.65(13) . . ?
O35 Mo8 Mo6 86.08(13) . . ?
O35 Mo8 O28 97.12(15) . . ?
O35 Mo8 O29 165.19(15) . . ?
O35 Mo8 O27 97.22(16) . . ?
O35 Mo8 O33 101.83(16) . . ?
O32 Mo8 Mo6 136.27(12) . . ?
O32 Mo8 O28 100.20(15) . . ?
O32 Mo8 O29 86.64(15) . . ?
O32 Mo8 O27 157.51(15) . . ?
O32 Mo8 O33 100.15(16) . . ?
O32 Mo8 O35 105.09(19) . . ?
O26 Mo10 O30 76.67(13) . . ?
O26 Mo10 O27 73.25(12) . . ?
O30 Mo10 O27 68.74(11) . . ?
O33 Mo10 O26 142.58(14) . . ?
O33 Mo10 O30 78.31(13) . . ?
O33 Mo10 O27 71.95(12) . . ?
O34 Mo10 O26 97.71(16) . . ?
O34 Mo10 O30 163.61(15) . . ?
O34 Mo10 O27 94.94(14) . . ?
O34 Mo10 O33 98.53(17) . . ?
O34 Mo10 O36 105.37(17) . . ?
O36 Mo10 O26 105.48(15) . . ?
O36 Mo10 O30 91.00(14) . . ?
O36 Mo10 O27 159.58(14) . . ?
O36 Mo10 O33 102.31(16) . . ?
O38 Mo11 N7 71.93(13) . . ?
O37 Mo11 O38 148.53(15) . . ?
O37 Mo11 N7 80.77(14) . . ?
O40 Mo11 O38 95.42(16) . . ?
O40 Mo11 O37 101.57(16) . . ?
O40 Mo11 N7 151.50(16) . . ?
O39 Mo11 O38 98.64(18) . . ?
O39 Mo11 O37 101.41(19) . . ?
O39 Mo11 O40 106.95(19) . . ?
O39 Mo11 N7 100.28(16) . . ?
O2 Mo1 O6 79.52(14) . . ?
O2 Mo1 N1 71.68(16) . . ?
O1 Mo1 O2 150.16(17) . . ?
O1 Mo1 O6 80.30(16) . . ?
O1 Mo1 N1 81.17(17) . . ?
O4 Mo1 O2 96.22(19) . . ?
O4 Mo1 O6 81.43(17) . . ?
O4 Mo1 O1 102.3(2) . . ?
O4 Mo1 N1 151.76(19) . . ?
N1 Mo1 O6 71.44(14) . . ?
O3 Mo1 O2 97.2(2) . . ?
O3 Mo1 O6 172.72(17) . . ?
O3 Mo1 O1 100.1(2) . . ?
O3 Mo1 O4 105.5(2) . . ?
O3 Mo1 N1 101.4(2) . . ?
Mo6 O21 Mo7 109.04(15) . . ?
Mo6 O21 Mo4 111.59(14) . . ?
Mo7 O21 Mo4 103.42(13) . . ?
Mo6 O28 Mo5 109.30(13) . . ?
Mo6 O28 Mo8 106.92(14) . . ?
Mo8 O28 Mo5 103.91(13) . . ?
Mo9 O25 Mo7 110.47(14) . . ?
Mo9 O25 Mo4 109.61(15) . . ?
Mo4 O25 Mo7 103.48(14) . . ?
Mo3 O15 Mo5 116.35(16) . . ?
Mo6 O20 Mo3 90.65(10) . . ?
Mo9 O20 Mo6 103.58(12) . . ?
Mo9 O20 Mo3 165.75(15) . . ?
Mo9 O20 Mo5 91.09(11) . . ?
Mo9 O20 Mo4 91.57(11) . . ?
Mo5 O20 Mo6 99.08(11) . . ?
Mo5 O20 Mo3 87.34(10) . . ?
Mo5 O20 Mo4 163.56(15) . . ?
Mo4 O20 Mo6 96.06(11) . . ?
Mo4 O20 Mo3 86.11(10) . . ?
C22 O8 Mo2 119.6(3) . . ?
Mo4 O14 Mo3 118.14(17) . . ?
Mo9 O29 Mo5 108.22(15) . . ?
Mo9 O29 Mo8 109.62(14) . . ?
Mo5 O29 Mo8 105.07(13) . . ?
C36 O38 Mo11 118.8(3) . . ?
Mo6 O13 Mo3 118.21(15) . . ?
Mo7 O26 Mo10 118.03(16) . . ?
Mo9 O30 Mo10 118.83(16) . . ?
Mo6 O27 Mo9 106.08(12) . . ?
Mo6 O27 Mo7 92.02(11) . . ?
Mo6 O27 Mo8 92.77(11) . . ?
Mo6 O27 Mo10 162.88(15) . . ?
Mo9 O27 Mo10 90.96(10) . . ?
Mo7 O27 Mo9 96.32(11) . . ?
Mo7 O27 Mo10 84.30(10) . . ?
Mo8 O27 Mo9 99.12(11) . . ?
Mo8 O27 Mo7 161.87(15) . . ?
Mo8 O27 Mo10 86.00(10) . . ?
Mo3 O11 Mo2 133.38(18) . . ?
Mo8 O33 Mo10 119.78(18) . . ?
C16 O7 Mo2 132.3(3) . . ?
C30 O37 Mo11 132.0(3) . . ?
C8 O2 Mo1 119.5(3) . . ?
Mo2 O6 Mo1 165.6(2) . . ?
N8 N7 Mo11 116.3(3) . . ?
C35 N7 Mo11 127.8(3) . . ?
C35 N7 N8 115.9(4) . . ?
C32 O41 C42 117.0(4) . . ?
N5 N4 Mo2 116.4(3) . . ?
C21 N4 Mo2 127.2(3) . . ?
C21 N4 N5 116.4(4) . . ?
C38 N9 H9 118.4 . . ?
C38 N9 C39 123.1(5) . . ?
C39 N9 H9 118.4 . . ?
C36 N8 N7 107.9(4) . . ?
C2 O1 Mo1 138.6(4) . . ?
C22 N5 N4 108.3(4) . . ?
C24 N6 H6 118.6 . . ?
C24 N6 C25 122.7(5) . . ?
C25 N6 H6 118.6 . . ?
C18 O10 C28 117.5(5) . . ?
N1 N2 H2 125.2 . . ?
C8 N2 H2 125.2 . . ?
C8 N2 N1 109.6(4) . . ?
C11 N3 H3 118.2 . . ?
C11 N3 C10 123.5(5) . . ?
C10 N3 H3 118.2 . . ?
O38 C36 C37 115.7(4) . . ?
N8 C36 O38 124.7(4) . . ?
N8 C36 C37 119.6(4) . . ?
H42D O42 H42E 104.3 . . ?
N9 C38 H38 120.1 . . ?
N9 C38 C37 119.8(5) . . ?
C37 C38 H38 120.1 . . ?
N2 N1 Mo1 115.4(3) . . ?
C7 N1 Mo1 129.3(4) . . ?
C7 N1 N2 115.2(4) . . ?
C34 C29 C35 120.0(4) . . ?
C30 C29 C35 121.9(4) . . ?
C30 C29 C34 118.1(4) . . ?
O8 C22 C23 116.4(4) . . ?
N5 C22 O8 123.4(4) . . ?
N5 C22 C23 120.2(4) . . ?
C23 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
C26 C27 C23 119.4(5) . . ?
C27 C23 C22 120.3(4) . . ?
C27 C23 C24 119.0(4) . . ?
C24 C23 C22 120.7(4) . . ?
N7 C35 C29 123.8(4) . . ?
N7 C35 H35 118.1 . . ?
C29 C35 H35 118.1 . . ?
O2 C8 C9 118.4(5) . . ?
N2 C8 O2 123.7(5) . . ?
N2 C8 C9 118.0(4) . . ?
C38 C37 C36 119.5(4) . . ?
C38 C37 C41 118.3(5) . . ?
C41 C37 C36 122.2(4) . . ?
N6 C24 C23 119.6(5) . . ?
N6 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C27 C26 H26 120.2 . . ?
C27 C26 C25 119.7(5) . . ?
C25 C26 H26 120.2 . . ?
O41 C32 C33 115.0(4) . . ?
O41 C32 C31 124.1(5) . . ?
C31 C32 C33 120.8(5) . . ?
C29 C34 H34 119.2 . . ?
C33 C34 C29 121.5(5) . . ?
C33 C34 H34 119.2 . . ?
N9 C39 H39 120.2 . . ?
N9 C39 C40 119.6(5) . . ?
C40 C39 H39 120.2 . . ?
N4 C21 H21 118.2 . . ?
N4 C21 C15 123.6(5) . . ?
C15 C21 H21 118.2 . . ?
C9 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C12 C13 C9 120.4(5) . . ?
C32 C33 H33 120.4 . . ?
C34 C33 C32 119.2(4) . . ?
C34 C33 H33 120.4 . . ?
N3 C11 H11 120.6 . . ?
N3 C11 C12 118.8(5) . . ?
C12 C11 H11 120.6 . . ?
O37 C30 C29 122.2(4) . . ?
O37 C30 C31 116.4(4) . . ?
C31 C30 C29 121.3(4) . . ?
N3 C10 H10 120.0 . . ?
N3 C10 C9 120.0(5) . . ?
C9 C10 H10 120.0 . . ?
C16 C15 C21 122.8(4) . . ?
C20 C15 C21 118.7(5) . . ?
C20 C15 C16 118.3(5) . . ?
C32 C31 C30 118.9(5) . . ?
C32 C31 H31 120.5 . . ?
C30 C31 H31 120.5 . . ?
C13 C9 C8 121.9(5) . . ?
C10 C9 C8 120.6(5) . . ?
C10 C9 C13 117.4(5) . . ?
C16 C17 H17 120.5 . . ?
C16 C17 C18 118.9(5) . . ?
C18 C17 H17 120.5 . . ?
N6 C25 C26 119.5(5) . . ?
N6 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C13 C12 H12 120.1 . . ?
C11 C12 C13 119.8(5) . . ?
C11 C12 H12 120.1 . . ?
O7 C16 C15 121.5(4) . . ?
O7 C16 C17 117.6(5) . . ?
C17 C16 C15 120.7(5) . . ?
C37 C41 H41 120.3 . . ?
C40 C41 C37 119.5(5) . . ?
C40 C41 H41 120.3 . . ?
C39 C40 C41 119.6(5) . . ?
C39 C40 H40 120.2 . . ?
C41 C40 H40 120.2 . . ?
O10 C18 C17 125.0(6) . . ?
O10 C18 C19 114.2(5) . . ?
C19 C18 C17 120.8(5) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 C18 119.7(5) . . ?
C20 C19 H19 120.2 . . ?
N1 C7 H7 118.3 . . ?
N1 C7 C1 123.3(5) . . ?
C1 C7 H7 118.3 . . ?
C15 C20 H20 119.2 . . ?
C19 C20 C15 121.5(5) . . ?
C19 C20 H20 119.2 . . ?
C7 C1 C6 118.9(6) . . ?
C2 C1 C7 124.5(6) . . ?
C2 C1 C6 116.5(6) . . ?
O1 C2 C1 121.9(5) . . ?
O1 C2 C3 115.8(6) . . ?
C3 C2 C1 122.3(7) . . ?
C1 C6 H6A 119.2 . . ?
C5 C6 C1 121.7(7) . . ?
C5 C6 H6A 119.2 . . ?
O41 C42 H42A 109.5 . . ?
O41 C42 H42B 109.5 . . ?
O41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C6 C5 H5 120.2 . . ?
C4 C5 C6 119.6(7) . . ?
C4 C5 H5 120.2 . . ?
C2 C3 H3A 120.5 . . ?
C2 C3 C4 119.1(7) . . ?
C4 C3 H3A 120.5 . . ?
O10 C28 H28A 109.5 . . ?
O10 C28 H28B 109.5 . . ?
O10 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C5 C4 C3 120.8(7) . . ?
C5 C4 O5B 98.1(9) . . ?
C5 C4 O5A 132.1(8) . . ?
C3 C4 O5B 139.9(10) . . ?
O5A C4 C3 106.8(8) . . ?
H14A C14A H14B 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
O5B C14A H14A 109.5 . . ?
O5B C14A H14B 109.5 . . ?
O5B C14A H14C 109.5 . . ?
C4 O5B C14A 104.2(14) . . ?
H14D C14B H14E 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
O5A C14B H14D 109.5 . . ?
O5A C14B H14E 109.5 . . ?
O5A C14B H14F 109.5 . . ?
C4 O5A C14B 111.1(9) . . ?
N10A C44A C43 177.4(11) . . ?
N10B C44B C43 175(3) . . ?
N11B C46B C45B 167(3) . . ?
C46B C45B H45A 109.5 . . ?
C46B C45B H45B 109.5 . . ?
C46B C45B H45C 109.5 . . ?
H45A C45B H45B 109.5 . . ?
H45A C45B H45C 109.5 . . ?
H45B C45B H45C 109.5 . . ?
H45D C45A H45E 109.5 . . ?
H45D C45A H45F 109.5 . . ?
H45E C45A H45F 109.5 . . ?
C46A C45A H45D 109.5 . . ?
C46A C45A H45E 109.5 . . ?
C46A C45A H45F 109.5 . . ?
N11A C46A C45A 166(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo6 Mo7 O26 Mo10 22.5(2) . . . . ?
Mo6 Mo8 O33 Mo10 -17.7(2) . . . . ?
Mo5 Mo9 O30 Mo10 78.1(2) . . . . ?
Mo7 Mo6 O13 Mo3 -73.7(2) . . . . ?
Mo2 O8 C22 N5 9.9(6) . . . . ?
Mo2 O8 C22 C23 -170.0(3) . . . . ?
Mo2 O7 C16 C15 32.6(7) . . . . ?
Mo2 O7 C16 C17 -150.8(4) . . . . ?
Mo2 N4 N5 C22 -3.8(5) . . . . ?
Mo2 N4 C21 C15 -7.7(7) . . . . ?
Mo8 Mo6 O13 Mo3 76.99(19) . . . . ?
Mo11 O38 C36 N8 -6.1(6) . . . . ?
Mo11 O38 C36 C37 174.7(3) . . . . ?
Mo11 O37 C30 C29 -37.5(7) . . . . ?
Mo11 O37 C30 C31 144.9(4) . . . . ?
Mo11 N7 N8 C36 3.9(5) . . . . ?
Mo11 N7 C35 C29 1.8(7) . . . . ?
Mo1 O2 C8 N2 -5.9(7) . . . . ?
Mo1 O2 C8 C9 174.8(3) . . . . ?
Mo1 O1 C2 C1 11.7(9) . . . . ?
Mo1 O1 C2 C3 -170.2(5) . . . . ?
Mo1 N1 C7 C1 -2.1(8) . . . . ?
O21 Mo6 O13 Mo3 -74.83(18) . . . . ?
O21 Mo7 O26 Mo10 54.2(3) . . . . ?
O21 Mo4 O14 Mo3 93.38(19) . . . . ?
O28 Mo6 O13 Mo3 77.18(18) . . . . ?
O28 Mo8 O33 Mo10 -49.9(4) . . . . ?
O25 Mo9 O30 Mo10 -74.40(19) . . . . ?
O25 Mo7 O26 Mo10 96.41(18) . . . . ?
O25 Mo4 O14 Mo3 50.5(3) . . . . ?
O15 Mo3 O11 Mo2 172.1(2) . . . . ?
O20 Mo6 O13 Mo3 1.02(15) . . . . ?
O20 Mo9 O30 Mo10 4.2(5) . . . . ?
O20 Mo3 O11 Mo2 -106.1(4) . . . . ?
O20 Mo4 O14 Mo3 20.09(17) . . . . ?
O8 Mo2 O6 Mo1 -44.5(8) . . . . ?
O8 C22 C23 C27 -11.1(7) . . . . ?
O8 C22 C23 C24 167.0(4) . . . . ?
O14 Mo3 O11 Mo2 -31.3(3) . . . . ?
O29 Mo9 O30 Mo10 78.14(19) . . . . ?
O29 Mo8 O33 Mo10 -92.1(2) . . . . ?
O38 C36 C37 C38 3.4(7) . . . . ?
O38 C36 C37 C41 -175.3(5) . . . . ?
O13 Mo3 O11 Mo2 -109.5(2) . . . . ?
O27 Mo6 O13 Mo3 3.6(4) . . . . ?
O27 Mo9 O30 Mo10 1.98(16) . . . . ?
O27 Mo7 O26 Mo10 23.40(17) . . . . ?
O27 Mo8 O33 Mo10 -20.56(18) . . . . ?
O16 Mo4 O14 Mo3 -179.00(19) . . . . ?
O23 Mo7 O26 Mo10 -66.5(2) . . . . ?
O22 Mo6 O13 Mo3 -179.14(17) . . . . ?
O7 Mo2 O6 Mo1 162.5(8) . . . . ?
O9 Mo2 O6 Mo1 55.0(8) . . . . ?
O12 Mo3 O11 Mo2 69.0(3) . . . . ?
O35 Mo8 O33 Mo10 74.3(2) . . . . ?
O31 Mo9 O30 Mo10 -178.39(17) . . . . ?
O17 Mo4 O14 Mo3 -70.9(2) . . . . ?
O37 C30 C31 C32 178.9(5) . . . . ?
O2 C8 C9 C13 -176.9(5) . . . . ?
O2 C8 C9 C10 -0.7(7) . . . . ?
O32 Mo8 O33 Mo10 -177.7(2) . . . . ?
O24 Mo7 O26 Mo10 -174.74(18) . . . . ?
N7 N8 C36 O38 1.0(6) . . . . ?
N7 N8 C36 C37 -179.8(4) . . . . ?
O41 C32 C33 C34 -177.0(5) . . . . ?
O41 C32 C31 C30 176.1(5) . . . . ?
N4 Mo2 O6 Mo1 -116.3(8) . . . . ?
N4 N5 C22 O8 -3.3(6) . . . . ?
N4 N5 C22 C23 176.6(4) . . . . ?
N4 C21 C15 C16 -13.0(8) . . . . ?
N4 C21 C15 C20 172.5(5) . . . . ?
N9 C38 C37 C36 179.8(4) . . . . ?
N9 C38 C37 C41 -1.5(7) . . . . ?
N9 C39 C40 C41 -0.2(9) . . . . ?
N8 N7 C35 C29 -177.5(4) . . . . ?
N8 C36 C37 C38 -175.9(4) . . . . ?
N8 C36 C37 C41 5.5(7) . . . . ?
O1 C2 C3 C4 -177.0(6) . . . . ?
N5 N4 C21 C15 175.9(4) . . . . ?
N5 C22 C23 C27 168.9(4) . . . . ?
N5 C22 C23 C24 -12.9(7) . . . . ?
O10 C18 C19 C20 -178.1(5) . . . . ?
N2 N1 C7 C1 175.8(5) . . . . ?
N2 C8 C9 C13 3.7(8) . . . . ?
N2 C8 C9 C10 179.9(5) . . . . ?
N3 C11 C12 C13 0.4(9) . . . . ?
N3 C10 C9 C8 -177.2(5) . . . . ?
N3 C10 C9 C13 -0.8(8) . . . . ?
C36 C37 C41 C40 178.6(5) . . . . ?
C38 N9 C39 C40 -1.5(9) . . . . ?
C38 C37 C41 C40 -0.1(8) . . . . ?
N1 N2 C8 O2 2.9(7) . . . . ?
N1 N2 C8 C9 -177.8(4) . . . . ?
N1 C7 C1 C2 -3.8(9) . . . . ?
N1 C7 C1 C6 178.9(5) . . . . ?
C29 C34 C33 C32 0.7(8) . . . . ?
C29 C30 C31 C32 1.3(8) . . . . ?
C22 C23 C24 N6 -178.6(4) . . . . ?
C27 C23 C24 N6 -0.5(7) . . . . ?
C27 C26 C25 N6 -0.3(8) . . . . ?
C23 C27 C26 C25 -0.8(8) . . . . ?
C35 N7 N8 C36 -176.7(4) . . . . ?
C35 C29 C34 C33 179.4(5) . . . . ?
C35 C29 C30 O37 2.1(7) . . . . ?
C35 C29 C30 C31 179.6(5) . . . . ?
C8 N2 N1 Mo1 1.1(5) . . . . ?
C8 N2 N1 C7 -177.1(5) . . . . ?
C37 C41 C40 C39 1.0(9) . . . . ?
C24 N6 C25 C26 1.1(8) . . . . ?
C26 C27 C23 C22 179.3(4) . . . . ?
C26 C27 C23 C24 1.2(7) . . . . ?
C34 C29 C35 N7 -169.7(5) . . . . ?
C34 C29 C30 O37 -175.3(4) . . . . ?
C34 C29 C30 C31 2.2(7) . . . . ?
C39 N9 C38 C37 2.4(8) . . . . ?
C21 N4 N5 C22 173.0(4) . . . . ?
C21 C15 C16 O7 3.5(7) . . . . ?
C21 C15 C16 C17 -173.0(5) . . . . ?
C21 C15 C20 C19 175.1(5) . . . . ?
C33 C32 C31 C30 -3.9(8) . . . . ?
C11 N3 C10 C9 -0.5(9) . . . . ?
C30 C29 C35 N7 13.0(7) . . . . ?
C30 C29 C34 C33 -3.1(7) . . . . ?
C10 N3 C11 C12 0.7(9) . . . . ?
C31 C32 C33 C34 2.9(8) . . . . ?
C9 C13 C12 C11 -1.7(9) . . . . ?
C17 C18 C19 C20 0.4(9) . . . . ?
C25 N6 C24 C23 -0.7(8) . . . . ?
C12 C13 C9 C8 178.2(5) . . . . ?
C12 C13 C9 C10 1.9(8) . . . . ?
C16 C15 C20 C19 0.4(8) . . . . ?
C16 C17 C18 O10 179.8(5) . . . . ?
C16 C17 C18 C19 1.5(8) . . . . ?
C18 C17 C16 O7 -179.1(5) . . . . ?
C18 C17 C16 C15 -2.5(8) . . . . ?
C18 C19 C20 C15 -1.3(9) . . . . ?
C7 C1 C2 O1 0.3(9) . . . . ?
C7 C1 C2 C3 -177.6(6) . . . . ?
C7 C1 C6 C5 176.8(6) . . . . ?
C20 C15 C16 O7 178.1(4) . . . . ?
C20 C15 C16 C17 1.6(7) . . . . ?
C1 C2 C3 C4 1.1(10) . . . . ?
C1 C6 C5 C4 0.9(10) . . . . ?
C2 C1 C6 C5 -0.7(9) . . . . ?
C2 C3 C4 C5 -0.9(11) . . . . ?
C2 C3 C4 O5B -165.4(12) . . . . ?
C2 C3 C4 O5A 173.1(7) . . . . ?
C6 C1 C2 O1 177.7(5) . . . . ?
C6 C1 C2 C3 -0.3(9) . . . . ?
C6 C5 C4 C3 0.0(11) . . . . ?
C6 C5 C4 O5B 169.9(8) . . . . ?
C6 C5 C4 O5A -172.3(9) . . . . ?
C42 O41 C32 C33 171.7(5) . . . . ?
C42 O41 C32 C31 -8.3(8) . . . . ?
C5 C4 O5B C14A 174.3(14) . . . . ?
C5 C4 O5A C14B 0.7(15) . . . . ?
C3 C4 O5B C14A -19(2) . . . . ?
C3 C4 O5A C14B -172.3(10) . . . . ?
C28 O10 C18 C17 -9.7(9) . . . . ?
C28 O10 C18 C19 168.8(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.231
_oxdiff_exptl_absorpt_empirical_full_min 0.597
# start Validation Reply Form
_vrf_PLAT315_exp_1663_auto       
;
PROBLEM: Singly Bonded Carbon Detected (H-atoms Missing).        C43 Check   
RESPONSE: This is a heavily disordered C-atom of the non-coordinated 
acetonitrile molecule.
;
_vrf_PLAT430_exp_1663_auto       
;
PROBLEM: Short Inter D...A Contact  O36      ..O40      .       2.80 Ang.  
 x,y,z  =      1_555 Check
Short Inter D...A Contact  O36      ..N7       .       2.85 Ang.  
x,y,z  =      1_555 Check 
RESPONSE: cis-MoO2 moiety is slightly skewed leading to closer than 
expected distances between neighboring atoms in the coordination sphere. 
However, no indications of errors in modelling the 
cis-MoO2 moiety were observed.
;
